反応式
[BH4-].[Li+].[F:3][C:4]1[C:9]([F:10])=[CH:8][CH:7]=[CH:6][C:5]=1[C@@H:11]1[CH2:21][CH2:20][C@@H:19]([O:22][Si:23]([CH:30]([CH3:32])[CH3:31])([CH:27]([CH3:29])[CH3:28])[CH:24]([CH3:26])[CH3:25])[C:14]2=[N:15][CH:16]=[CH:17][CH:18]=[C:13]2[C:12]1=[O:33]>COC1CCCC1>[F:3][C:4]1[C:9]([F:10])=[CH:8][CH:7]=[CH:6][C:5]=1[C@@H:11]1[CH2:21][CH2:20][C@@H:19]([O:22][Si:23]([CH:27]([CH3:29])[CH3:28])([CH:30]([CH3:32])[CH3:31])[CH:24]([CH3:25])[CH3:26])[C:14]2=[N:15][CH:16]=[CH:17][CH:18]=[C:13]2[C@H:12]1[OH:33]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 0 °C
実験手順
Lithium borohydride (0.982 g, 45.1 mmol) was added to a cyclopentyl methyl ether (30 mL) solution of (6S,9R)-6-(2,3-difluorophenyl)-9-(triisopropylsilyloxy)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-one (5.0224 g, 11.27 mmol) at 0° C. under N2. The reaction mixture was stirred at 0° C. for 2 hours and then an addition 4 hours at room temperature. The reaction was quenched by adding methanol. The reaction mixture was stirred for 0.5 hour. The solvent was mostly removed via vacuum and the crude material was taken up in ethyl acetate, which was washed with water three times. Flash column by ethyl acetate in hexane from 0 to 10% gave the desired product (3.28 g, 65%).
後処理
- additionan addition 4 hours at room temperature
- customThe reaction was quenched
- additionby adding methanol
- stirringThe reaction mixture was stirred for 0.5 hour
- customThe solvent was mostly removed via vacuum
- washwhich was washed with water three times
出典と根拠
- ORDレコード
- ord-613adbb88c844232aca16582d503ae0a
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759372B2
関連ノート
読み込み中…