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Ethanol → 5,6-Dichloro-2-(4-carboxy-2-ethoxyphenyl)benzimidazole hydrochloride

HRID 1352661
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반응식

HRID 1352661 반응식
Cl.[Cl:2][C:3]1[C:22]([Cl:23])=[CH:21][C:6]2[N:7]=[C:8]([C:10]3[CH:15]=[CH:14]C(C#N)=[CH:12][C:11]=3[O:18][CH2:19][CH3:20])[NH:9][C:5]=2[CH:4]=1.[OH-:24].[Na+].[CH2:26]([OH:28])[CH3:27]>>[ClH:2].[Cl:2][C:3]1[C:22]([Cl:23])=[CH:21][C:6]2[N:7]=[C:8]([C:10]3[CH:15]=[CH:14][C:27]([C:26]([OH:24])=[O:28])=[CH:12][C:11]=3[O:18][CH2:19][CH3:20])[NH:9][C:5]=2[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 211011675,6-Dichloro-2-(4-cyano-2-ethoxyphenyl)benzimidazole hydrochloride

생성물 1

HCID 211011635,6-Dichloro-2-(4-carboxy-2-ethoxyphenyl)benzimidazole hydrochloride수율 70%

실험 절차

A mixture of 5,6-dichloro-2-(4-cyano-2-ethoxyphenyl)benzimidazole hydrochloride (16.3 g, 44.2 mmol), prepared as in Preparation 12, 32% NaOH (40 ml) in ethanol (100 ml) was refluxed for 8 h. After cooling to room temperature the organic solvent was removed under vacuum and the aqueous phase was acidified with 37% HCl, stirred for 1 h. The solid was filtered, washed with water (100 ml) and dried at 50° C. under vacuum to give 12 g of the title compound as a light brown powder (yield 70%), mp>250° C.

후처리

  1. temperaturewas refluxed for 8 h
  2. customwas removed under vacuum
  3. filtrationThe solid was filtered
  4. washwashed with water (100 ml)
  5. customdried at 50° C. under vacuum

출처 및 근거

ORD 기록
ord-283fbcb77ef7408faa690bc1d65e7bd0
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07220769B2

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