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发 送 文 章     CAS号[938-73-8]生产工艺-止痛药Ethenzamide [留言][评论][收藏] 收信地址     填写收信人的电子邮箱 邮件主题     填写邮件主题 邮件内容  <p class="MsoNormal" align="center" style="font-size:medium;white-space:normal;text-align:center;"> <span lang="EN-US" style="font-size:16pt;">CAS</span><span style="font-size:16pt;font-family:宋体;">号</span><span lang="EN-US" style="font-size:16pt;">[938-73-8]</span><span style="font-size:16pt;font-family:宋体;">生产工艺</span><span lang="EN-US" style="font-size:16pt;">-</span><span style="font-size:16pt;font-family:宋体;">止痛药</span><span lang="EN-US" style="font-size:16pt;">Ethenzamide<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">名】</span><span lang="EN-US" style="font-size:12pt;">Benzamide, 2-ethoxy-</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">Beil. 10, 93; E2, 58; E4, 175.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【用途】止痛药</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">（日）《有机化合物辞典》，有机合成化学协会编，</span><span lang="EN-US" style="font-size:12pt;">1985</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 158</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">エトキシベンズアミド。</span><span lang="EN-US" style="font-size:12pt;">2-Ethoxybenzamide; Ethenzamide</span><span style="font-size:12pt;font-family:宋体;">；</span><span lang="EN-US" style="font-size:12pt;">CA [938-73-8]</span><span style="font-size:12pt;font-family:宋体;">，化审</span><span lang="EN-US" style="font-size:12pt;"> 3 – 1679</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">  C<sub>9</sub>H<sub>11</sub>NO<sub>2</sub> = 165.19</span><span style="font-size:12pt;font-family:宋体;">，</span><span style="font-size:12pt;font-family:宋体;">结构式：略，</span><span lang="EN-US" style="font-size:12pt;">M.P. 132 – 134</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">10</span><span style="font-size:12pt;font-family:宋体;">局，</span><span lang="EN-US" style="font-size:12pt;">P</span><span lang="EN-US" style="font-size:12pt;">. 127</span><span style="font-size:12pt;font-family:宋体;">，</span><span style="font-size:12pt;font-family:宋体;">白色の结晶または结晶性粉末，無味，無臭。クロロホルムに易溶，热汤，エ</span><span lang="EN-US" style="font-size:12pt;">-</span><span style="font-size:12pt;font-family:宋体;">テルに难溶，水に不溶。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【制法】サリチルアミドとクロロエタンを加压下，加热する</span><span lang="EN-US" style="font-size:12pt;"> [Pol. Pat. 47,822 (1963)]. </span><span style="font-size:12pt;font-family:宋体;">【用途】镇痛剂。【毒性】</span><span lang="EN-US" style="font-size:12pt;">LD50</span><span style="font-size:12pt;font-family:宋体;">（マウス，经口）</span><span lang="EN-US" style="font-size:12pt;">1160 mg/kg [G. A. Starmer et al., Toxicol. Appl. Pharmacol., 19, 20 (1971)]</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">候乐山主编《中国精细化工产品集</span><span style="font-size:12pt;"> <span lang="EN-US">– </span></span><span style="font-size:12pt;font-family:宋体;">原料及中间体</span><span lang="EN-US" style="font-size:12pt;">10396</span><span style="font-size:12pt;font-family:宋体;">种》，中国化工信息中心出版，</span><span lang="EN-US" style="font-size:12pt;">2006</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 815</span><span style="font-size:12pt;font-family:宋体;">，摘录如下：</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【中文名】邻乙氧基苯甲酰胺；乙基水杨酸；止痛灵；</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">乙氧基苯甲酰胺；乙柳酰胺；乙基水杨酰胺。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【英文名】</span><span lang="EN-US" style="font-size:12pt;">0-Ethoxybenzamide; Ethylsalicylamide; Ethbenzamide; Etenzamide; Lu-camid; 2-Ethoxybenzenecarbonamide; Salicylamide; o-Ethyl ether; 2-Ethoxy benzamide. <o:p></o:p></span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【</span><span style="font-size:12pt;font-family:宋体;">分子式】</span><span lang="EN-US" style="font-size:12pt;">C<sub>9</sub>H<sub>11</sub>NO<sub>2</sub>  <o:p></o:p></span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【</span><span style="font-size:12pt;font-family:宋体;">分子量】</span><span lang="EN-US" style="font-size:12pt;">165.19 <o:p></o:p></span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【</span><span lang="EN-US" style="font-size:12pt;">CAS#</span><span style="font-size:12pt;font-family:宋体;">】</span><span lang="EN-US" style="font-size:12pt;">938-73-8<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【物质登记状态】未登记</span><span lang="EN-US" style="font-size:12pt;"> <o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【</span><span lang="EN-US" style="font-size:12pt;">RTECS</span><span style="font-size:12pt;font-family:宋体;">编号】</span><span lang="EN-US" style="font-size:12pt;">CV4900000<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【熔点】</span><span lang="EN-US" style="font-size:12pt;">132~134</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【产品性状】白色或类白色结晶性粉末。易溶于氯仿，乙醇，丙酮，难溶于水，乙醚。几乎无臭，无味。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【生产方法】由水杨酰胺</span><span lang="EN-US" style="font-size:12pt;"> [65-45-2]</span><span style="font-size:12pt;font-family:宋体;">经乙基化而得。将水杨酰胺，固体氢氧化钠，乙醇置于反应锅内，密闭升温至</span><span lang="EN-US" style="font-size:12pt;">60 – 70</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，搅拌</span><span lang="EN-US" style="font-size:12pt;">30 min</span><span style="font-size:12pt;font-family:宋体;">，冷却至</span><span lang="EN-US" style="font-size:12pt;">30</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，加入溴乙烷</span><span lang="EN-US" style="font-size:12pt;"> [74-96-4]</span><span style="font-size:12pt;font-family:宋体;">，再密闭升温至</span><span lang="EN-US" style="font-size:12pt;">80 – 100</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，压力不超过</span><span lang="EN-US" style="font-size:12pt;">0.2 MPa</span><span style="font-size:12pt;font-family:宋体;">，反应</span><span lang="EN-US" style="font-size:12pt;">3 h</span><span style="font-size:12pt;font-family:宋体;">。降至常压，</span><span lang="EN-US" style="font-size:12pt;">pH</span><span style="font-size:12pt;font-family:宋体;">应在</span><span lang="EN-US" style="font-size:12pt;">8.5</span><span style="font-size:12pt;font-family:宋体;">以上。趁热过滤，滤渣溴化钠回收。滤液蒸出大部分乙醇后，加蒸馏水析出白色结晶。过滤，水洗至中性，干燥，得邻乙氧基苯甲酰胺。收率约</span><span lang="EN-US" style="font-size:12pt;">75%</span><span style="font-size:12pt;font-family:宋体;">。也可采用氯乙烷</span><span lang="EN-US" style="font-size:12pt;"> [75-00-3]</span><span style="font-size:12pt;font-family:宋体;">，但需要较高压力。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【抄注】无资料来源，应该是抄自</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">内部资料</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">！以下，略。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">张大国编著《精细有机单元反应合成技术手册》，化学工业出版社出版，</span><span lang="EN-US" style="font-size:12pt;">2014</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 250</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">051027  </span><span style="font-size:12pt;font-family:宋体;">邻乙氧基苯甲酰胺（止痛灵）。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【分子式】</span><span lang="EN-US" style="font-size:12pt;">C<sub>9</sub>H<sub>11</sub>NO<sub>2</sub></span><span style="font-size:12pt;font-family:宋体;">；</span><span style="font-size:12pt;font-family:宋体;">【分子量】</span><span lang="EN-US" style="font-size:12pt;">165.19</span><span style="font-size:12pt;font-family:宋体;">；</span><span style="font-size:12pt;font-family:宋体;">【性质】白色或类白色结晶性粉末，几乎无臭，无味。易溶于氯仿，乙醇，丙酮，难溶于水，乙醚。熔点</span><span lang="EN-US" style="font-size:12pt;">131 – 134</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">。【用途】解热止痛药。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【制法】反应式：略。</span><span lang="EN-US" style="font-size:12pt;">A</span><span style="font-size:12pt;font-family:宋体;">法。配料比：水杨酰胺</span><span lang="EN-US" style="font-size:12pt;">[65-45-2] : </span><span style="font-size:12pt;font-family:宋体;">溴乙烷</span><span lang="EN-US" style="font-size:12pt;">[74-96-4] : </span><span style="font-size:12pt;font-family:宋体;">固碱</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">：乙醇</span><span lang="EN-US" style="font-size:12pt;"> =1 </span><span style="font-size:12pt;font-family:宋体;">：</span><span lang="EN-US" style="font-size:12pt;">0.9 </span><span style="font-size:12pt;font-family:宋体;">：</span><span lang="EN-US" style="font-size:12pt;">0.35 </span><span style="font-size:12pt;font-family:宋体;">：</span><span lang="EN-US" style="font-size:12pt;">2</span><span style="font-size:12pt;font-family:宋体;">。将水杨酰胺，固碱，乙醇加入反应罐，密闭升温至</span><span lang="EN-US" style="font-size:12pt;">60 – 70</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，保温</span><span lang="EN-US" style="font-size:12pt;">30 min</span><span style="font-size:12pt;font-family:宋体;">。冷却至</span><span lang="EN-US" style="font-size:12pt;">45</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">以下，加入溴乙烷</span><span lang="EN-US" style="font-size:12pt;">[74-96-4]</span><span style="font-size:12pt;font-family:宋体;">，密闭搅拌升温至</span><span lang="EN-US" style="font-size:12pt;">80 – 100</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，压力不超过</span><span lang="EN-US" style="font-size:12pt;">0.2 MPa</span><span style="font-size:12pt;font-family:宋体;">，保温</span><span lang="EN-US" style="font-size:12pt;">3 h</span><span style="font-size:12pt;font-family:宋体;">。降至常压，</span><span lang="EN-US" style="font-size:12pt;">pH</span><span style="font-size:12pt;font-family:宋体;">值应在</span><span lang="EN-US" style="font-size:12pt;">8.5</span><span style="font-size:12pt;font-family:宋体;">以上，热滤，用少量乙醇洗，抽干。滤液回收乙醇，加蒸馏水，析出结晶。过滤，水洗至中性，甩干，干燥，得止痛灵。收率</span><span lang="EN-US" style="font-size:12pt;">73 – 75%</span><span style="font-size:12pt;font-family:宋体;">。（无资料来源，应该是抄自</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">内部资料</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">！而且</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">制法</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">与候乐山的资料相同！）</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">B</span><span style="font-size:12pt;font-family:宋体;">法。将</span><span lang="EN-US" style="font-size:12pt;">50 ml 95%</span><span style="font-size:12pt;font-family:宋体;">乙醇，</span><span lang="EN-US" style="font-size:12pt;">70 g</span><span style="font-size:12pt;font-family:宋体;">氢氧化钠，水杨酰胺</span><span lang="EN-US" style="font-size:12pt;">200 g</span><span style="font-size:12pt;font-family:宋体;">加入反应瓶，搅拌，温热溶解后，降至室温。加入</span><span lang="EN-US" style="font-size:12pt;">5 g</span><span style="font-size:12pt;font-family:宋体;">三乙基苄基氯化铵</span><span lang="EN-US" style="font-size:12pt;"> [56-37-1]</span><span style="font-size:12pt;font-family:宋体;">（抄注：相转移催化剂，已上网！）和</span><span lang="EN-US" style="font-size:12pt;">175 g</span><span style="font-size:12pt;font-family:宋体;">溴乙烷</span><span lang="EN-US" style="font-size:12pt;">[74-96-4]</span><span style="font-size:12pt;font-family:宋体;">，于</span><span lang="EN-US" style="font-size:12pt;">80 – 85</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，压力为</span><span lang="EN-US" style="font-size:12pt;">0.15 – 0.17MPa</span><span style="font-size:12pt;font-family:宋体;">反应</span><span lang="EN-US" style="font-size:12pt;">3 h</span><span style="font-size:12pt;font-family:宋体;">。降至</span><span lang="EN-US" style="font-size:12pt;">70</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，滤去溴化钠，蒸去乙醇，加入</span><span lang="EN-US" style="font-size:12pt;">80</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;"> 2000 ml</span><span style="font-size:12pt;font-family:宋体;">的水，降至室温，过滤结晶，水洗至中性，干燥得邻乙氧基苯甲酰胺粗品</span><span lang="EN-US" style="font-size:12pt;">233 g</span><span style="font-size:12pt;font-family:宋体;">。收率</span><span lang="EN-US" style="font-size:12pt;">96.7%</span><span style="font-size:12pt;font-family:宋体;">。用</span><span lang="EN-US" style="font-size:12pt;">50%</span><span style="font-size:12pt;font-family:宋体;">乙醇重结晶得精品。精制率为</span><span lang="EN-US" style="font-size:12pt;">97.2%</span><span style="font-size:12pt;font-family:宋体;">。（其中</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号为本人所加。）</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【参考文献】中国医药工业杂志，</span><span lang="EN-US" style="font-size:12pt;">2000, 31 (2): 56</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【寄言】老有所为，</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">科技资料的收集与整理</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">，只希望能有点利用价值。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">陈忠源</span><span lang="EN-US" style="font-size:12pt;"> 2021</span><span style="font-size:12pt;font-family:宋体;">年</span><span lang="EN-US" style="font-size:12pt;">8</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">2</span><span style="font-size:12pt;font-family:宋体;">日，星期一</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /><br /><br />本文地址：<a href="http://www.陈忠源化学文库.cn/Article.asp?ID=10001612" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001612</a>   填写邮件内容   邮件签名     填写邮件签名 发信地址     填写发信人的电子邮箱 　验证码     填写验证码，单击即可刷新验证码   发送协议 ·欢迎使用本站在线文章发送系统。 ·不得使用本站在线发送邮件系统发送垃圾邮件、广告邮件。 ·如果收信人地址或其服务器出现错误，可能无法成功发送。 ·如果有什么问题，或者意见建议，请联系[网站管理员]。

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