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Lithium hydroxide, monohydrate → 2-[(4-Bromo-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazole-7-carboxylic acid

HRID 2235575
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HRID 2235575 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([NH:9][C:10]2[N:14]([CH3:15])[C:13]3[C:16]([C:20]([O:22]C)=[O:21])=[CH:17][CH:18]=[CH:19][C:12]=3[N:11]=2)=[C:4]([O:24][CH3:25])[CH:3]=1.O.[OH-].[Li+]>O1CCCC1.O>[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([NH:9][C:10]2[N:14]([CH3:15])[C:13]3[C:16]([C:20]([OH:22])=[O:21])=[CH:17][CH:18]=[CH:19][C:12]=3[N:11]=2)=[C:4]([O:24][CH3:25])[CH:3]=1
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 68582017Methyl 2-[(4-bromo-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazole-7-carboxylate

생성물 1

HCID 685813862-[(4-Bromo-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazole-7-carboxylic acid수율 77.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran
용매

실험 절차

To a solution of 150 mg (0.371 mmol) of methyl 2-[(4-bromo-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazole-7-carboxylate in 5 mL of tetrahydrofuran and 2.5 mL of water was added 156 mg (3.71 mmol) of lithium hydroxide monohydrate and the reaction was stirred at room temperature overnight and concentrated in vacuo. The thus obtained residue was diluted with water and carefully adjusted to pH 4-5 using 1 N aqueous hydrochloric acid. The resulting solids were filtered, washed with water and dried under high vacuum to give 112 mg (77%) of the title compound as white solids.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe thus obtained residue was diluted with water
  3. filtrationThe resulting solids were filtered
  4. washwashed with water
  5. customdried under high vacuum

출처 및 근거

ORD 기록
ord-6f1c0168e83d47f392775de72ada0e22
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07714009B2

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