3,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)aniline synthesis

Yield:-

Reaction Conditions:

in N,N-dimethyl-formamide at 80 - 150;Large scale;

Steps:

4 4, addition process:
600 kg of dimethylformamide (DMF) was added to the addition kettle,200 kg of 2,6-dichloro-4-aminophenol was added with stirring,Dissolved and heated to 80 ° C,And then through the addition of tetrafluoroethylene gas addition reaction.After the reaction,The material after the addition reaction was distilled at 150 ° C.At the end of the distillation,First turn off the steamer jacket steam,Exhaust the remaining steam in the kettle jacket,Cooling with cooling water,So that the kettle temperature dropped to 100 ,And then close the receiver vacuum valve,Using nitrogen protection piercing,A crude product of 3,5-dichloro-4- (1,1,2,2-tetrafluoroethoxy) aniline was obtained.5 to 8% of the residue can be removed by distillation,Distilled residue is additionally treated.Analysis of 3,5-dichloro-4- (1,1,2,2-tetrafluoroethoxy) aniline (referred to as: fluoride ether) crude quality of the various components:3,5-dichloro-4- (1,1,2,2-tetrafluoroethoxy) aniline was 94%DMF is 5% and difluoroether is 1%.

References:

Yangzhou Tianchen Fine Chemical Co., Ltd.;Shen, Guoyun;Wang, Chen;Pan, Mingsheng;Liu, Runxing;Chen, Zhongcheng;Miao, Youchang;Zhang, Chaogang;Zhang, Xiaofeng;Luo, Rui;Wang, Zhengjun;Cai, Lei CN106278911, 2017, A Location in patent:Paragraph 0013; 0035; 0036; 0037; 0038; 0039