Sodium Hydroxide → 2-{2,6-Dichloro-3-[(2,2-dimethyl-propionylamino)-methyl]-phenylamino}-6-[3,3-difluoro-pyrrolidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid

HRID 1189648노트

반응식

HRID 1189648 반응식
C[O:2][C:3]([C:5]1[C:31]([N:32]2[CH2:36][CH2:35][C:34]([F:38])([F:37])[CH2:33]2)=[CH:30][C:8]2[N:9]([CH3:29])[C:10]([NH:12][C:13]3[C:18]([Cl:19])=[CH:17][CH:16]=[C:15]([CH2:20][NH:21][C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])[C:14]=3[Cl:28])=[N:11][C:7]=2[CH:6]=1)=[O:4].[OH-].[Na+]>CCO>[Cl:28][C:14]1[C:15]([CH2:20][NH:21][C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:16][CH:17]=[C:18]([Cl:19])[C:13]=1[NH:12][C:10]1[N:9]([CH3:29])[C:8]2[CH:30]=[C:31]([N:32]3[CH2:36][CH2:35][C:34]([F:37])([F:38])[CH2:33]3)[C:5]([C:3]([OH:4])=[O:2])=[CH:6][C:7]=2[N:11]=1

참가 물질

4

반응 조건

온도
50 °C

실험 절차

A mixture of 2-{2,6-dichloro-3-[(2,2-dimethyl-propionylamino)-methyl]-phenylamino}-6-[3,3-difluoro-pyrrolidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid methyl ester (2.37 g, 4.17 mmol), 2 N NaOH-solution (9.8 ml) and EtOH (20 ml) is stirred for 1 h at rt and for 2 h at 50° C. and concentrated. Water is added and it is filtered. The filtrate is acidified with 4N HCl (pH 5) and the precipitate is filtered, washed with water and dried.

후처리

  1. concentrationconcentrated
  2. additionWater is added
  3. filtrationit is filtered
  4. filtrationthe precipitate is filtered
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-bb81945c7e944761818072c6d1ca62a8
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674113B2

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