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

HRID 1090860ノート

反応式

HRID 1090860 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
120 °C

実験手順

200 ml of tetrahydrofuran and 50 g of 2,4,6-trifluorobenzotrifluoride were initially introduced into a stainless steel autoclave and it was pressurized using 30 ml of liquid ammonia. Subsequently, the mixture was heated at 120° C. for 6 hours with stirring. After cooling and releasing the pressure, the reaction mixture was subjected to a fractional distillation. 15 g of 2-amino-4,6-difluoro-benzotrifluoride were obtained at a boiling point of 57° to 58° C. at 12 mbar. After a small intermediate run, 32 g of 2,6-difluoro-4-amino-benzotrifluoride passed over at a boiling point of 103° to 105° C. at 16 mbar. The melting point of the 2,6-difluoro-4-amino-benzotrifluoride obtained was 66° C.

後処理

  1. temperatureAfter cooling
  2. distillationthe reaction mixture was subjected to a fractional distillation

出典と根拠

ORDレコード
ord-1c921bf62c2e444f8dfb82ffd7375839
出典データセット
uspto-grants-1992_01
特許番号
US05082971

反応ノート

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