Ammonia → 3,5-Difluoro-2-(trifluoromethyl)aniline

HRID 1710108노트

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HRID 1710108 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4](F)[C:3]=1[C:10]([F:13])([F:12])[F:11].[NH3:14]>O1CCCC1>[NH2:14][C:4]1[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[C:3]=1[C:10]([F:13])([F:12])[F:11]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 27340301,3,5-Trifluoro-2-(trifluoromethyl)benzene

생성물 1

HCID 27834103,5-Difluoro-2-(trifluoromethyl)aniline

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
120 °C

실험 절차

In a stainless steel autoclave, 200 ml of tetrahydrofuran and 50 g of 2,4,6-trifluorobenzotrifluoride are introduced, and 30 ml of liquid ammonia are pressed on. The mixture is then heated at 120° C. for 6 hours, with stirring. The reaction mixture is cooled, the pressure is released, and the mixture is subjected to fractional distillation. At a boiling point of 57° to 58° C. at 12 mbar, 15 g of 2-amino-4,6-difluoro-benzotrifluoride are obtained. After a small intermediate cut, 32 g of 2,6-difluoro-4-amino-benzotrifluoride distil over at a boiling point of 103° to 105° C. at 16 mbar. Melting point of the resultant 2,6-difluoro-4-amino-benzotrifluoride: 66° C.

후처리

  1. temperatureThe reaction mixture is cooled
  2. distillationthe mixture is subjected to fractional distillation

출처 및 근거

ORD 기록
ord-43ddf55f690142f189a5584047384029
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04952601

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