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

HRID 1189705노트

반응식

HRID 1189705 반응식
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

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 679575112-{2,6-Dichloro-3-[aminomethyl]-phenylamino}-6-[4-trifluoromethyl-piperidinyl]-1-methyl-1H-benzimidazole-5-carboxylic acid ethyl ester

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1ab53163a30c4e09a115f1f966775f28
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674113B2

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