反応式
[Li+].[OH-].C([O:6][C@@H:7]1[CH2:31][CH2:30][C@@:29]2([CH3:32])[C@H:9]([CH2:10][CH2:11][C@@H:12]3[C@@H:28]2[CH2:27][C@H:26]([OH:33])[C@@:25]2([CH3:34])[C@H:13]3[CH2:14][CH2:15][C@@H:16]2[C@H:17]([CH3:24])[CH2:18][CH2:19][C:20]([O:22]C)=[O:21])[CH2:8]1)(=O)C>O.C1COCC1.CO>[CH3:24][C@@H:17]([C@@H:16]1[C@@:25]2([CH3:34])[C@@H:26]([OH:33])[CH2:27][C@@H:28]3[C@@:29]4([CH3:32])[CH2:30][CH2:31][C@@H:7]([OH:6])[CH2:8][C@H:9]4[CH2:10][CH2:11][C@H:12]3[C@@H:13]2[CH2:14][CH2:15]1)[CH2:18][CH2:19][C:20]([OH:22])=[O:21]参加物
6
反応条件
- 温度
- 50 °C
実験手順
A solution of LiOH (187 mg, 4.4 mmol) in H2O (2.0 mL) was added to a solution of compound 2.1a (500 mg, 1.11 mmol) in THF (8 mL) and MeOH (8 mL). The resulting mixture was stirred for 3-4 h 50° C. Upon complete disappearance of the starting material by TLC, the reaction mixture was concentrated under vacuum. A mixture of water (10 mL) and 3 N HCl (1 mL) were combined and cooled to 0° C. and then added to the crude product. After stirring for 1 h at 0° C., the precipitated solids were filtered and then washed with water (10 mL) and hexane (20 mL). Drying under vacuum at room temperature provided deoxycholic acid (DCA, 400 mg, 91% yield) as a white solid.
後処理
- concentrationUpon complete disappearance of the starting material by TLC, the reaction mixture was concentrated under vacuum
- additionA mixture of water (10 mL) and 3 N HCl (1 mL)
- temperaturecooled to 0° C.
- additionadded to the crude product
- stirringAfter stirring for 1 h at 0° C.
- filtrationthe precipitated solids were filtered
- washwashed with water (10 mL) and hexane (20 mL)
- customDrying under vacuum at room temperature
出典と根拠
- ORDレコード
- ord-fecebffaf3544226aaf62c7a0dbc2e1a
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367852B2
関連ノート
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