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| CAS号 [20304-70-5] 生产工艺。 9-氨基-7-乙氧基-3-硝基吖啶 | |
CAS号 [20304-70-5] 生产工艺。 9-氨基-7-乙氧基-3-硝基吖啶
CAS名：Acridine, 5-amino-2-nitro-7-ethoxy- 历史参考文献：待检索。
用途：医药，利凡诺。LookChem网登录生产与经营单位3家。BIOS 1155, 15-16. 9-Chloro-7-ethoxy-3-nitroacridine and 9-Amino-7-ethxoy-3-nitroacridine. 英国人译自德文（无资料来源）。 反应式：本人有加注。暂未找到德文原件。  Starting materials: 25 kg. Nitro ethoxy acid。 100 kg. xylol。 16.88 kg. Phosphorous oxychloride。 72.0 kg. Phenol。 20.8 kg. Aqueous ammonia. The ring closure is carried out in an enameled iron kettle from which vacuum distillations may be made. Two such units were present. The phosphorous oxychloride is sucked up to a container at the top, and the xylol in stored above and run in as required. The Nitro-ethoxy acid is heated with 100 kg xylol to a temperature of 75℃. In 20 min. (twenty minutes) 8.44 kg. of phosphorous oxychloride is then allowed enter and the temperature rises to 100℃ in about 2 hours. A further 8.44 kg. of phosphorous oxychloride is then added and the temperature rises to 110℃., where it is maintained for one hour. The reaction mixture is then heated to 130-135℃.and the xylol distilled off using slightly reduced pressure. About 80 kg. of distillate are obtained. The contents of the vessel are allowed to cool at 50℃. and 72 kg. of phenol are added. The mixture is then again warmed until distillation takes place and about 16 kg of a mixture of xylol and ammonia water are collected. The temperature is afterwards maintained at 130-140℃. for half an hour then cooled to 70℃. and treated with 100 kg. of spirit. After being well stirred the mixture is filtered with suction. The residue is washed with 25 kg. of spirits, then added to 175 l. of water and 4.8 kg. of hydrochloric acid, the mixture is heated to boiling and the solid filtered off and washed with water. Yield = approximately 20 kg. mp. 275-277℃. 抄注：[74859-51-1] 已上网，侯乐山 主编《中国精细化工产品集 – 原料及中间体10396种》，2006年出版。 p. 1379. 2-[(4-乙氧基苯基)氨基]-4-硝基苯甲酸。生产厂：上海第一生化药业公司上海第一制药厂生产。应该是，上述中间体到利凡诺也会有生产，但书中未提到。再说，上述资料国内有进口，没有利用是我们应该思考的问题。 如果有读者可以提供这类资料，我是深表谢意，其实，我手头有一些BIOS是原沈阳院总工，李光天同志送给我的，在这里也再次表示谢意！同时，也可以说明这类资料不仅仅是只有染料及其中间体，请见已上网的资料。应该承认这类资料是已过时的历史资料（但是读者不一定全知道！）。 致谢： 上述中间体的CAS号是读者：徐英 同志提供，使我能在今天上网，将英国人的译文供读者参考，在此深表谢意！其实，BIOS 1155 我没有收藏，这是以前手工抄录的资料，如果读者能提供这类资料的复印件，我会继续按CAS号编写上网。再次谢谢读者！因为下面的CAS号[442-16-0]和[1837-57-6] 的生产工艺我未抄录。 陈忠源 2018年11月2日星期五。
文章作者：陈忠源 |