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发 送 文 章     CAS号[94-34-8]生产工艺N-甲基-N-氰乙基苯胺 [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;">[94-34-8]</span><span style="font-size:16pt;font-family:宋体;">生产工艺</span><span lang="EN-US" style="font-size:16pt;">N-</span><span style="font-size:16pt;font-family:宋体;">甲基</span><span lang="EN-US" style="font-size:16pt;">-N-</span><span style="font-size:16pt;font-family:宋体;">氰乙基苯胺</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 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;">Propanenitrile, 3-(methylphenyl)amino-   Beil. 12. E1, 267; E3, 934; E4, 890. </span><span style="font-size:12pt;font-family:宋体;">其中摘录</span><span lang="EN-US" style="font-size:12pt;">E4, 890</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;">结构式：略。</span><span style="font-size:12pt;"><span lang="EN-US"><o:p></o:p></span></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">分子式：</span><span lang="EN-US" style="font-size:12pt;">C<sub>10</sub>H<sub>12</sub>N<sub>2</sub><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;">分子量：</span><span lang="EN-US" style="font-size:12pt;">160.22  <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：染料中间体（</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;">24</span><span style="font-size:12pt;font-family:宋体;">；</span><span lang="EN-US" style="font-size:12pt;">C.I.</span><span style="font-size:12pt;font-family:宋体;">碱性红</span><span lang="EN-US" style="font-size:12pt;">14</span><span style="font-size:12pt;font-family:宋体;">；</span><span lang="EN-US" style="font-size:12pt;"> C.I.</span><span style="font-size:12pt;font-family:宋体;">分散橙</span><span lang="EN-US" style="font-size:12pt;">25:1</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;">Beil. 12, E4, 890 </span><span style="font-size:12pt;font-family:宋体;">抄录如下（不再翻译！）：</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 style="font-size:12pt;font-family:宋体;">制备方法】</span><span lang="EN-US" style="font-size:12pt;">Aus N-Methyl-anilin und Acrylonitril (Heininger. J. Org. Chem. 22(1957) 1213, 1216; Allison et al., Soc. 1954, 403, 406).<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">Beim Erhitzen von N,N-Diäthyl-β-alanin-nitril mit N-Methyl-anilin-hydrochlorid (Bates et al., Soc. 1956, 388, 390).<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">Kp 0.6: 127 – 1280; n23.5/D : 1.5590 (Ba et al.).  Kp 0.05: 116 - 1170 (Al. et al.).<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;">上海市有机化学工业公司《染料生产工艺汇编》</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;">，</span><span lang="EN-US" style="font-size:12pt;">1976</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">P. 540</span><span style="font-size:12pt;font-family:宋体;">，</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">阳离子艳红</span><span lang="EN-US" style="font-size:12pt;">5GN</span><span style="font-size:12pt;font-family:宋体;">。其中</span><span lang="EN-US" style="font-size:12pt;">[94-34-8]</span><span style="font-size:12pt;font-family:宋体;">的生产工艺。</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 style="font-size:12pt;font-family:宋体;">【抄注】本</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;">是采用二次世界大战后，美国人的</span><span lang="EN-US" style="font-size:12pt;">“FIAT”</span><span style="font-size:12pt;font-family:宋体;">和英国人的</span><span lang="EN-US" style="font-size:12pt;">“BIOS”</span><span style="font-size:12pt;font-family:宋体;">格式，他们是将所得到德国</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">生产工艺</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">编写出版图书，获得利益。当然，也方便了读者！所以，国内在</span><span lang="EN-US" style="font-size:12pt;">60 – 70</span><span style="font-size:12pt;font-family:宋体;">年代，也采用这一方法，从而编写出</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">内部出版物</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">，如《染料生产工艺汇编》、《塑料生产工艺汇编》、《医药生产工艺汇编》等。这已是历史！因为是</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">内部</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">资料，所以一般读者是不可能得到的！当然，国内也早已有人将所得到的</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;">以公开出版物的形式出版，问题是他们没有说是抄录的！最典型的例子：</span><span lang="EN-US" style="font-size:12pt;">XXX </span><span style="font-size:12pt;font-family:宋体;">主编《精细有机化学品技术手册》，科学出版社出版，</span><span lang="EN-US" style="font-size:12pt;">1992</span><span style="font-size:12pt;font-family:宋体;">年。问题是至今还有人，以不同方式，重复抄录出版！</span><span style="font-size:12pt;font-family:宋体;">资料中【反应式】：略。（其中参与反应的化合物，本人已加有</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号）。</span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">在反应锅内，加入</span><span lang="EN-US" style="font-size:12pt;">107</span><span style="font-size:12pt;font-family:宋体;">公斤</span><span lang="EN-US" style="font-size:12pt;">N-</span><span style="font-size:12pt;font-family:宋体;">甲基苯胺</span><span lang="EN-US" style="font-size:12pt;"> [100-61-8]</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">4</span><span style="font-size:12pt;font-family:宋体;">公斤冰醋酸，</span><span lang="EN-US" style="font-size:12pt;">0.5</span><span style="font-size:12pt;font-family:宋体;">公斤结晶醋酸铜和</span><span lang="EN-US" style="font-size:12pt;">1</span><span style="font-size:12pt;font-family:宋体;">公斤苯酚。加热至</span><span lang="EN-US" style="font-size:12pt;">120</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，通氮气排除空气后，在</span><span lang="EN-US" style="font-size:12pt;">135 – 150</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;">1.5</span><span style="font-size:12pt;font-family:宋体;">公斤</span><span lang="EN-US" style="font-size:12pt;">/</span><span style="font-size:12pt;font-family:宋体;">厘米</span><span lang="EN-US" style="font-size:12pt;">2</span><span style="font-size:12pt;font-family:宋体;">压力下，分批加入</span><span lang="EN-US" style="font-size:12pt;">63.6</span><span style="font-size:12pt;font-family:宋体;">公斤丙烯腈</span><span lang="EN-US" style="font-size:12pt;"> [107-13-1]</span><span style="font-size:12pt;font-family:宋体;">。在</span><span lang="EN-US" style="font-size:12pt;">140 – 155</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;">10</span><span style="font-size:12pt;font-family:宋体;">小时。冷却至</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;">，吸至真空蒸馏锅进行蒸馏，收集</span><span lang="EN-US" style="font-size:12pt;">155 – 175</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;">/5</span><span style="font-size:12pt;font-family:宋体;">毫米汞柱之馏分。得</span><span lang="EN-US" style="font-size:12pt;">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;">（</span><span lang="EN-US" style="font-size:12pt;">β-</span><span style="font-size:12pt;font-family:宋体;">氰乙基）苯胺</span><span lang="EN-US" style="font-size:12pt;">142</span><span style="font-size:12pt;font-family:宋体;">公斤。收率：</span><span lang="EN-US" style="font-size:12pt;">88.7%</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;">张澍声《精细化工中间体及产品生产工艺》，沈阳院出版，</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. 475</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">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;">（</span><span lang="EN-US" style="font-size:12pt;">β-</span><span style="font-size:12pt;font-family:宋体;">氰乙基）苯胺。</span><span style="font-family:宋体;font-size:12pt;">【抄注】其生产工艺完全抄自《染料生产工艺汇编》，当然，未说明资料来源！本人不再抄录。</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. 422</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;">095007. N-</span><span style="font-size:12pt;font-family:宋体;">甲基</span><span lang="EN-US" style="font-size:12pt;">-N-(β-</span><span style="font-size:12pt;font-family:宋体;">氰乙基</span><span lang="EN-US" style="font-size:12pt;">)</span><span style="font-size:12pt;font-family:宋体;">苯胺。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【性质】无色液体。沸点</span><span lang="EN-US" style="font-size:12pt;">155 – 175</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;">0.6 kPa</span><span style="font-size:12pt;font-family:宋体;">）。【制法】经本人核对，也是抄自《染料生产工艺汇编》，同样未说明资料来源！不再抄录。</span><span lang="EN-US" style="font-size:12pt;">[</span><span style="font-size:12pt;font-family:宋体;">该书是</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">版权所有</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">的！</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 style="font-size:12pt;font-family:宋体;">国外产品规格：（</span><span lang="EN-US" style="font-size:12pt;">Henkel</span><span style="font-size:12pt;font-family:宋体;">）</span><span lang="EN-US" style="font-size:12pt;">Organic Intermediates, Emery (R) 5722,  N-Cyanoethyl-M-methyl Aniline CAS Number 94-34-8, 1993</span><span style="font-size:12pt;font-family:宋体;">年。</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;">  Form </span><span style="font-size:12pt;font-family:宋体;">外观：</span><span lang="EN-US" style="font-size:12pt;"> Brown liquid                            Flash Point, C.O.C. </span><span style="font-size:12pt;font-family:宋体;">闪点：</span><span lang="EN-US" style="font-size:12pt;">143</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;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  Boiling Point, 20 mmHg </span><span style="font-size:12pt;font-family:宋体;">沸点：</span><span lang="EN-US" style="font-size:12pt;">176</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;">         Specific Gravity, 20</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;">比重：</span><span lang="EN-US" style="font-size:12pt;">1.05.<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;">  Analysis%                                / Typical   / Specifications<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  Acetic Acid by Acid Value            / 0.4       / 1.5 max.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  G.L.C. Analysis %  </span><span style="font-size:12pt;font-family:宋体;">气液色谱</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;">  N-Methyl Aniline  [100-61-8]       / 0.2       / 1.0 max.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  N,N-Dimethyl Aniline [121-69-7]  / 0.3       / 1.0 max.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  Low Boiler                                 / 0.2         -<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  N-Methyl Acetanilide [579-10-2]  / 0.7         -<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  N-Cyanoethyl-N-Methyl Aniline    / 97.8       / 95 min.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  High Boiler                                / 0.4         -<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">  Applications   C.I. Basic Orange 24; C.I. Basic Red 14;  C.I. Disperse Orange 25:1<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;">7</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">18</span><span style="font-size:12pt;font-family:宋体;">日星期日。</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=10001603" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001603</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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