Sodium Hydroxide → 2-(2,6-dichlorophenyl)-1-methyl-1H-benzoimidazole-5-carboxylic acid

HRID 1514921ノート

反応式

HRID 1514921 の反応式
C([O:3][C:4]([C:6]1[CH:23]=[CH:22][C:9]2[N:10]([CH3:21])[C:11]([C:13]3[C:18]([Cl:19])=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:20])=[N:12][C:8]=2[CH:7]=1)=[O:5])C.[OH-].[Na+]>CCO>[Cl:20][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]([Cl:19])[C:13]=1[C:11]1[N:10]([CH3:21])[C:9]2[CH:22]=[CH:23][C:6]([C:4]([OH:5])=[O:3])=[CH:7][C:8]=2[N:12]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 669657182-(2,6-dichlorophenyl)-1-methyl-1H-benzoimidazole-5-carboxylic acid ethyl ester

生成物 1

HCID 638902812-(2,6-dichlorophenyl)-1-methyl-1H-benzoimidazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

To a suspension of 2-(2,6-dichlorophenyl)-1-methyl-1H-benzoimidazole-5-carboxylic acid ethyl ester (400 mg) in EtOH (8 mL) was added 1.0 N NaOH (2.0 mL) and the mixture was stirred at 60° C. for 90 min. The ethanol was removed under reduced pressure and water (10 mL) was added. Any insoluble material was filtered and 2.0N HCl (2.0 mL) was added to the filtrate. The resulting precipitate was filtered, washed with water and dried under reduced pressure to give 2-(2,6-dichlorophenyl)-1-methyl-1H-benzoimidazole-5-carboxylic acid as a white solid, mp>250° C.; MS (m/z) 321 (M+1).

後処理

  1. customThe ethanol was removed under reduced pressure and water (10 mL)
  2. additionwas added
  3. filtrationAny insoluble material was filtered
  4. addition2.0N HCl (2.0 mL) was added to the filtrate
  5. filtrationThe resulting precipitate was filtered
  6. washwashed with water
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7079db5bfa2b494cba51ccec150ca648
出典データセット
uspto-grants-2012_07
特許番号
US08222248B2

反応ノート

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