CAS号 [61537-49-3] 生产工艺    3-羟基-4’-甲基二苯胺

CAS名: Phenol, 3-[(4-methylphenyl)amino]-       历史参考文献: Beil. 13, 412.

用途; 医药：酚妥拉明（CAS号[50-60-2]）中间体。染料：酸性紫15。   反应类别: 缩合。

BIOS 986, 231-233.（=胶卷PB 77764）。No. 138. 3-Hydroxy-4’-methyl-diphenylamine (oxybase) (m-Oxyphenyl-p-toluidine).

反应式: 本人有加注，译者译自德文（无资料来源 – 实际是PB 25602, 295-305的摘译）。生产厂I.G. Ludwigshafen =BASF .

Plant: 略。文中（1）到（6）为设备号。
Process:  (A)  Condensation :

For the first batch of a complain charge to the still (1) 1,400 kg. resorcin (= 46% of the resorcine plus toluidine ) and 19 kg. sulfanilic acid.  Then suck in 1,640 kg. of p-toluidine (= 54% of the resorcine plus toluidine).  In serial production the fresh addition of resorcine amounts to about 1,230 kg.  Heat to 120℃.  The resorcine melts.  Then start the agitator and heat in 4 hours to 180-190℃.  From this point water with some toluidine and resorcine distils through the sight-glass into the receiver (6).  Distillate temperature 98-102℃.  Adjust the dephlogmator cooling water to 60℃.  In the course of 12 hours raise the kettle temperature to 235-240℃.  Then the distillation of water ceases the distillate temperature falls and the condensation is finished.  Shut off the agitator and heating and let the contents of the kettle cool during about 10 houra to about 200℃.  190-210 kg. water (95-100% of the calculated amount) distils over.  With the first batch the water is accompanied by about 30 kg. of a mixture of resorcine and toluidine.  In serial production one obtains 60-70 kg. of a mixture of these with an average content of 55% p-toluidine, 5% resorcine and 40% oxybase.  The condenser and pipeline to the receiver also contains some oxybase separated from the water.  Discard the water.  This recovered oil mixture is reused when sufficieny has cooumulated the charge being adjusted to the amount and composition of the recovery.

(B)  Distillation:  略。

Capacity:  略。   Quality: 87℃. setting point.     Production: 历年产量，略。

张澍声 《精细化工中间体工业生产技术》 1996年。 P. 3-羟基-4’-甲基二苯胺。 译自BIOS 986, 231.  不再抄录。

PB 25602, 295-305. “Oxybase”  3-Hydroxyphenyl-toluidine. 德文生产工艺，共11页。缩微胶卷已原样拷贝。

本人过去的方法是用放大镜放大，逐一抄录。今天已现代化了（本人无此条件），所以不再抄录！

致读者：

上网已2年多，知道读者不需要通过本网页来学习外文，需要的是解决实际问题。本网页只是CA的补充（只是历史资料），也应该向CA学习，因为该索引从来没有全文抄录，只是摘要而已。

至于PB报告，本人想法也有点多余。当然，能提供相应的CAS号，只是本人的理想，是否有用，也要通过实际考验。总之，以后不再全文抄录！除非有多余的页面。实际上，本人可以抄录的历史资料已不多了，部分只是一些产品标题，特别是商品名，要找出其对应的CAS号，不看原件是不可能做到的！当然，有人可以提供历史资料原件，还是可以继续！

本网页只能是一个“产品索引”。

奋斗是幸福的！A retired (more than 25 years) old man 更是幸福 + 幸福 ！只是希望我的努力能对读者有点用！

陈忠源 2018年2月21日（年初六）