Hydrochloric Acid → (E)-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-hydroxy-acrylic acid

HRID 2116679

反応式

HRID 2116679 の反応式
C(N/[C:5](=[CH:9]/[C:10]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[C:13]([NH2:20])=[C:12]([Cl:21])[CH:11]=1)/[C:6]([OH:8])=[O:7])(=O)C.Cl.[OH2:23]>CN1C(=O)CCC1>[NH2:20][C:13]1[C:14]([C:16]([F:19])([F:18])[F:17])=[CH:15][C:10](/[CH:9]=[C:5](/[OH:23])\[C:6]([OH:8])=[O:7])=[CH:11][C:12]=1[Cl:21]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 66941463(E)-2-acetylamino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-acrylic acid

生成物 1

HCID 67043136(E)-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-hydroxy-acrylic acid

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
130 °C

実験手順

51.0 g (158 mmol) (E)-2-acetylamino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-acrylic acid, dissolved in 408 ml NMP, were combined with 612 ml aqueous 4-molar hydrochloric acid solution and stirred for 3 hours at a bath temperature of 130° C. stirred. The reaction mixture was cooled and poured onto 2000 ml of water with stirring. The precipitate formed was suction filtered, washed with 400 ml of water, dried overnight at 60° C. and recrystallised from 1000 ml boiling toluene.

後処理

  1. stirringstirred
  2. temperatureThe reaction mixture was cooled
  3. stirringwith stirring
  4. customThe precipitate formed
  5. filtrationfiltered
  6. washwashed with 400 ml of water
  7. customdried overnight at 60° C.
  8. customrecrystallised from 1000 ml

出典と根拠

ORDレコード
ord-1865c91b6b5b40e686352f2c345f66c0
出典データセット
uspto-grants-2008_10
特許番号
US07439237B2

関連ノート

読み込み中…