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

HRID 2235575
ノート
印刷プレビュー

反応式

HRID 2235575 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6f1c0168e83d47f392775de72ada0e22
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07714009B2

反応ノート

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