Hydrochloric Acid → Sodium Chloride

HRID 592331노트

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HRID 592331 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]3[NH:14][C:15](=[O:22])[N:16]([CH2:17][C:18]([OH:21])([CH3:20])[CH3:19])[C:12]=3[CH:11]=[C:10]([C:23]([O:25]C)=[O:24])[CH:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+:28].[ClH:29]>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]3[NH:14][C:15](=[O:22])[N:16]([CH2:17][C:18]([OH:21])([CH3:20])[CH3:19])[C:12]=3[CH:11]=[C:10]([C:23]([OH:25])=[O:24])[CH:9]=2)=[CH:4][CH:3]=1.[Cl-:29].[Na+:28]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 66690107Methyl 7-(4-fluorophenyl)-3-(2-hydroxy-2-methylpropyl)-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate

생성물 2

HCID 5234Sodium Chloride수율 982.1%HCID 666901397-(4-Fluorophenyl)-3-(2-hydroxy-2-methylpropyl)-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
100 °C

실험 절차

To a solution of methyl 7-(4-fluorophenyl)-3-(2-hydroxy-2-methylpropyl)-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate (80.0 mg, 0.223 mmol) in MeOH (0.446 mL) was added sodium hydroxide (0.446 mL, 1M, 0.446 mmol). Reaction heated in the microwave at 100° C. for 15 min. More sodium hydroxide (0.446 mL, 1M, 0.446 mmol) added and heated an additional 20 min in the microwave at 100° C. HCl (0.446 mL, 2M in ether, 0.892 mmol) was added and the reaction mixture was concentrated to give the title compound with four equivalents of sodium chloride (128 mg): LC-MS [M+1]=345.3.

후처리

  1. customReaction
  2. temperatureheated an additional 20 min in the microwave at 100° C
  3. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-c433d0da69a548df9a4ed10db856b054
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238647B2

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