Sodium Hydroxide → 2-{2,6-Dichloro-3-[aminomethyl]-phenylamino}-6-[4-trifluoromethyl-piperidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid

HRID 1189705ノート

反応式

HRID 1189705 の反応式
C([O:3][C:4]([C:6]1[C:26]([N:27]2[CH2:32][CH2:31][CH:30]([C:33]([F:36])([F:35])[F:34])[CH2:29][CH2:28]2)=[CH:25][C:9]2[N:10]([CH3:24])[C:11]([NH:13][C:14]3[C:19]([Cl:20])=[CH:18][CH:17]=[C:16]([CH2:21][NH2:22])[C:15]=3[Cl:23])=[N:12][C:8]=2[CH:7]=1)=[O:5])C.[OH-].[Na+]>CO>[Cl:23][C:15]1[C:16]([CH2:21][NH2:22])=[CH:17][CH:18]=[C:19]([Cl:20])[C:14]=1[NH:13][C:11]1[N:10]([CH3:24])[C:9]2[CH:25]=[C:26]([N:27]3[CH2:32][CH2:31][CH:30]([C:33]([F:36])([F:35])[F:34])[CH2:29][CH2:28]3)[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 679575112-{2,6-Dichloro-3-[aminomethyl]-phenylamino}-6-[4-trifluoromethyl-piperidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid ethyl ester

生成物 1

HCID 679573152-{2,6-Dichloro-3-[aminomethyl]-phenylamino}-6-[4-trifluoromethyl-piperidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-{2,6-dichloro-3-[aminomethyl]-phenylamino}-6-[4-trifluoromethyl-piperidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid ethyl ester (5.83 g, 10 mmol), 50% aq NaOH-solution (25 ml) and MeOH (100 ml) is stirred for 2.5 h at rt. The mixture is concentrated and slowly added to ice-cooled 12 M aq HCl (39.5 mL). Then aq NaHCO3 solution is added (to pH 8) and the resulting precipitate is collected by filtration and dried.

後処理

  1. concentrationThe mixture is concentrated
  2. additionslowly added to ice-
  3. temperaturecooled 12 M aq HCl (39.5 mL)
  4. additionThen aq NaHCO3 solution is added (to pH 8)
  5. filtrationthe resulting precipitate is collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-1ab53163a30c4e09a115f1f966775f28
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…