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 1189648ノート

反応式

HRID 1189648 の反応式
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

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 679572902-{2,6-Dichloro-3-[(2,2-dimethyl-propionylamino)-methyl]-phenylamino}-6-[3,3-difluoro-pyrrolidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid methyl ester

生成物 1

HCID 679572792-{2,6-Dichloro-3-[(2,2-dimethyl-propionylamino)-methyl]-phenylamino}-6-[3,3-difluoro-pyrrolidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-bb81945c7e944761818072c6d1ca62a8
出典データセット
uspto-grants-2014_03
特許番号
US08674113B2

反応ノート

読み込み中…