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

HRID 2116679

반응식

HRID 2116679 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
130 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1865c91b6b5b40e686352f2c345f66c0
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07439237B2

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