CAS号 [74859-51-1] 生产工艺。 2-[(4-乙氧基苯基)氨基]-4-硝基苯甲酸
CAS名:Benzoic acid, 2-[(4-ethoxyphenyl)amino]-4-nitro- 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8家,
BIOS 1155, 14. Nitro-ethoxydiphenylamino-carboxylic acid. 英国人译自德文(无资料来源)。
反应式:本人有加注,是以前手工抄录的资料,暂未找到德文原件。
Starting materials: 75 kg p-Phenetidine. 36.8 kg Sodium acetate. 27.3 kg 2-Chloro-4-nitrobenzoic acid.
0.054 kg Copper bronze.
The phenetidine is warmed to 600 in an enameled iron vessel fitted with an electric stirrer. The sodium acetate is added, then the chloronitrobenzoic acid and the copper bronze and the mass is heated externally with steam for 3 hours. The temperature is 110 – 115℃ and reflux condenser is used. The product is blown over into a wooden vat which contains 78 kg of hydrochloric acid and 200 liters of water. The precipitate is filtered off with suction on a porous stoneware filter The crude product is again stirred up with 100 liters of water and filtered off. It is then dissolved up (about 60 kg moist) in 650 liters of water and 28 kg of caustic soda (600Be’) with direct steam heating. The solution is filtered through sand after treatment with charcoal and the acid precipitated with 12 kg of hydrochloric acid at 90℃. The pure acid is filtered off with suction on a stoneware filter, washed with 50 liters of water and dried at 90℃. Yield: Approximately 33 kg. mp: 235-236℃.
抄注:以上英文,本人暂不翻译。
侯乐山 主编 《中国精细化工产品集 – 原料及中间体10396种》 2006年. P. 1379.
中国化工信息中心 全国精细化工原料及中间体行业协作组 出版 《版权所有 未经允许 不得翻印》
2-[(4-乙氧基苯基)氨基]-4-硝基苯甲酸。
英文名;2-[(4-Ethoxyphenyl)amino]-4-nitrobenzoic acid.
分子式:C15H14N2O5 分子量:302.29 CAS:74858-51-1 物质登记状态:未登记。
产品性状:结晶化合物。
生产方法:用2-氯-4-硝基苯甲酸与对氨基苯乙醚在铜粉催化下缩合制得。
用途:利凡诺的中间体。
生产厂:上海第一生化药业公司上海第一制药厂。
抄注:无资料来源,无产品结构式。
再次抄录加注:
国内早有进口资料,未充分利用只能说明国内对这类资料没有引起足够的重视,本人再次提出,供读者参考!如果还有点用,希望能将德文原件,PB报告利用起来。上面只是英国人的译文。
陈忠源 2018年10月26日星期五。 本文地址:http://www.陈忠源化学文库.cn/Article.asp?ID=10000839