Lithium hydroxide, monohydrate → 4-Hydroxy-1-methyl-1H-indole-2-carboxylic acid
反応式
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:12]([O:14]CC)=[O:13])[N:6]2[CH3:11].O[Li].O.OS([O-])(=O)=O.[K+]>C1COCC1.O>[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:12]([OH:14])=[O:13])[N:6]2[CH3:11]参加物
6
実験手順
To a solution of ethyl 4-hydroxy-1-methyl-1H-indole-2-carboxylate (0.20 g) in THF (20 mL) was added LiOH.H2O (0.1 g) in water (20 mL) and the resulting two phase solution was stirred at room temperature under nitrogen for 4 hr. The reaction mixture was acidified with KHSO4 and the product was extracted into EtOAc, washed with brine, dried over MgSO4, and concentrated. The residue was chromatographed over silica gel with a mixture of EtOAc and hexane to give 0.12 g of the title compound. MS ES (M++H)=192.
後処理
- extractionthe product was extracted into EtOAc
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe residue was chromatographed over silica gel with a mixture of EtOAc and hexane
出典と根拠
- ORDレコード
- ord-e810149489c74e7fa991868e3fe86a55
- 出典データセット
- uspto-grants-2008_07
- 特許番号
- US07402604B2
反応ノート
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