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发 送 文 章     CAS号[1757-72-8]生产工艺，2-苯基-1-甲基吲哚-3-醛 [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;">[1757-72-8]</span><span style="font-size:16pt;font-family:宋体;">生产工艺，</span><span lang="EN-US" style="font-size:16pt;">2-</span><span style="font-size:16pt;font-family:宋体;">苯基</span><span lang="EN-US" style="font-size:16pt;">-1-</span><span style="font-size:16pt;font-family:宋体;">甲基吲哚</span><span lang="EN-US" style="font-size:16pt;">-3-</span><span style="font-size:16pt;font-family:宋体;">醛</span><span lang="EN-US" style="font-size:16pt;"><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;">1H-Indole-3-carboxaldehyde, 1-methyl-2-phenyl-<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】碱性染料中间体。</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" align="left" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">BIOS1153.322-2</span><span style="font-size:12pt;font-family:宋体;">（</span><span lang="EN-US" style="font-size:12pt;">=</span><span style="font-size:12pt;font-family:宋体;">胶卷</span><span lang="EN-US" style="font-size:12pt;">PB 85687</span><span style="font-size:12pt;font-family:宋体;">）</span><span lang="EN-US" style="font-size:12pt;"> 2-Phenyl-1-methylindole-3-aldehyde (3-Aldehydo-2-phenyl-1-methylindole) (Leverkusen). </span><span style="font-size:12pt;font-family:宋体;">德文原件暂未找到，反应式：略。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">（</span><span style="font-size:12pt;font-family:宋体;">参与反应的化合物，本人已加上</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号。）</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;">【</span><span lang="EN-US" style="font-size:12pt;">Plant</span><span style="font-size:12pt;font-family:宋体;">】</span><span lang="EN-US" style="font-size:12pt;">Copper reaction vessel with heating and cooling jacket</span><span lang="EN-US" style="font-size:12pt;">, </span><span lang="EN-US" style="font-size:12pt;">C.I. tank for drown-out</span><span lang="EN-US" style="font-size:12pt;">, </span><span lang="EN-US" style="font-size:12pt;">Separator, C.I. Still</span><span lang="EN-US" style="font-size:12pt;">.</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;">【</span><span lang="EN-US" style="font-size:12pt;">Process</span><span style="font-size:12pt;font-family:宋体;">】</span><span lang="EN-US" style="font-size:12pt;">The reaction vessel is charged with 30.6 kgs of POCl3 [10025-87-3] and 27 kgs of methylformanilide [93-61-8] and the mixture warmed slightly to initiate the reaction. After 2 hours’ agitation, the mixture is diluted by the addition of 150 kgs o-dichlorobenzene and cooled to about 5</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;">. Then with agitation and with cooling to prevent the temperature from rising above 10</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;">, 41.4 kgs 2-phenyl-1-methylindole [3558-24-5] are added in small portions.  After stirring for 15 min. at room temperature, the batch is blown into 200 kgs of ice and 100 kgs of 400Be’ caustic liquor.  After good agitation the mixture is allowed to settle in a separator and the o-dichlorobenzene layer blown to a still. o-Dichlorobenzene and recovered methylaniline distill first followed by the 2-phenyl-1-methylindole-3-aldehyde [1757-72-8] at 229</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;"> at 4 mm pressure. Yield = 43.5 kgs = 92.5% theory.<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;">张澍声编译《精细化工中间体工业生产技术</span><span lang="EN-US" style="font-size:12pt;">–BIOS FIAT PB Report</span><span style="font-size:12pt;font-family:宋体;">》，染料工业编辑部出版</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">1996</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 272</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;">【产品名称】</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">苯基</span><span lang="EN-US" style="font-size:12pt;">-1-</span><span style="font-size:12pt;font-family:宋体;">甲基吲哚</span><span lang="EN-US" style="font-size:12pt;">-3-</span><span style="font-size:12pt;font-family:宋体;">醛；</span><span style="font-size:12pt;font-family:宋体;">【</span><span style="font-size:12pt;font-family:宋体;">产品结构式】略（其中</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号为本人所添加）。【制法】在铜反应釜中加入</span><span lang="EN-US" style="font-size:12pt;">30.6 kgs</span><span style="font-size:12pt;font-family:宋体;">磷酰氯</span><span lang="EN-US" style="font-size:12pt;">[10025-87-3] </span><span style="font-size:12pt;font-family:宋体;">和</span><span lang="EN-US" style="font-size:12pt;">27 kgs N-</span><span style="font-size:12pt;font-family:宋体;">甲基</span><span lang="EN-US" style="font-size:12pt;">-N-</span><span style="font-size:12pt;font-family:宋体;">甲酰苯胺</span><span lang="EN-US" style="font-size:12pt;">[93-61-8]</span><span style="font-size:12pt;font-family:宋体;">，混合物稍微温热以启动反应。搅拌</span><span lang="EN-US" style="font-size:12pt;">2</span><span style="font-size:12pt;font-family:宋体;">小时后，混合物加入</span><span lang="EN-US" style="font-size:12pt;">150 kgs </span><span style="font-size:12pt;font-family:宋体;">邻二氯苯进行稀释，冷却到约</span><span lang="EN-US" style="font-size:12pt;">5</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">。然后在搅拌和冷却下以小批量加入</span><span lang="EN-US" style="font-size:12pt;">41.4 kgs 1-</span><span style="font-size:12pt;font-family:宋体;">甲基</span><span lang="EN-US" style="font-size:12pt;">-2-</span><span style="font-size:12pt;font-family:宋体;">苯基吲哚</span><span lang="EN-US" style="font-size:12pt;"> [3555-24-5]</span><span style="font-size:12pt;font-family:宋体;">，防止温度超过</span><span lang="EN-US" style="font-size:12pt;">0</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">（抄注：错了，原文是</span><span lang="EN-US" style="font-size:12pt;">10</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">）。在室温搅拌</span><span lang="EN-US" style="font-size:12pt;">15</span><span style="font-size:12pt;font-family:宋体;">分钟后，反应物压入</span><span lang="EN-US" style="font-size:12pt;">200 kgs</span><span style="font-size:12pt;font-family:宋体;">冰和</span><span lang="EN-US" style="font-size:12pt;">100 kgs 35% </span><span style="font-size:12pt;font-family:宋体;">氢氧化钠溶液中。经很好搅拌后，混合物在分离器中静置分层，将邻二氯苯送入蒸馏釜中，首先蒸馏出邻二氯苯和回收的甲基苯胺，然后在</span><span lang="EN-US" style="font-size:12pt;">229</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">和</span><span lang="EN-US" style="font-size:12pt;">4 mm</span><span style="font-size:12pt;font-family:宋体;">压力下蒸馏出</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">苯基</span><span lang="EN-US" style="font-size:12pt;">-1-</span><span style="font-size:12pt;font-family:宋体;">甲基吲哚</span><span lang="EN-US" style="font-size:12pt;">-3-</span><span style="font-size:12pt;font-family:宋体;">醛</span><span lang="EN-US" style="font-size:12pt;"> [1757-72-8]</span><span style="font-size:12pt;font-family:宋体;">。得到</span><span lang="EN-US" style="font-size:12pt;">43.5 kgs</span><span style="font-size:12pt;font-family:宋体;">产品，收率</span><span lang="EN-US" style="font-size:12pt;">92.5%</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;">(</span><span style="font-size:12pt;font-family:宋体;">本产品又名</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">醛基</span><span lang="EN-US" style="font-size:12pt;">-2-</span><span style="font-size:12pt;font-family:宋体;">苯基</span><span lang="EN-US" style="font-size:12pt;">-1-</span><span style="font-size:12pt;font-family:宋体;">甲基吲哚。译自</span><span lang="EN-US" style="font-size:12pt;">BIOS1153, 323</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;">)</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;">何岩彬主编《染料品种大全》，沈阳出版社出版，</span><span lang="EN-US" style="font-size:12pt;">2018</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 2007</span><span style="font-size:12pt;font-family:宋体;">，</span><span style="font-size:12pt;font-family:宋体;">《染料中间体及可合成的染料》。</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;">【中文名称】</span><span lang="EN-US" style="font-size:12pt;">1-</span><span style="font-size:12pt;font-family:宋体;">甲基</span><span lang="EN-US" style="font-size:12pt;">-2-</span><span style="font-size:12pt;font-family:宋体;">苯基吲哚</span><span lang="EN-US" style="font-size:12pt;">-3-</span><span style="font-size:12pt;font-family:宋体;">甲醛。</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;">【可合成的染料】</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">碱性橙</span><span lang="EN-US" style="font-size:12pt;">22.<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;">【抄注】手头暂未见国内有人</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">翻译</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">本产品的合成工艺！</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;">3</span><span style="font-size:12pt;font-family:宋体;">日，星期二</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /><br /><br />本文地址：<a 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