반응식
[Si:1]([O:18][C@H:19]1[C:24](=[CH2:25])[C@@H:23]([F:26])[CH2:22]/[C:21](=[CH:27]\[C:28](OCC)=[O:29])/[CH2:20]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C>ClCCl.C1(C)C=CC=CC=1>[Si:1]([O:18][C@H:19]1[C:24](=[CH2:25])[C@@H:23]([F:26])[CH2:22]/[C:21](=[CH:27]\[CH2:28][OH:29])/[CH2:20]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- -78 °C
실험 절차
The compound of Example 13G (40 mg, 0.09 mmol) was dissolved in 1 mL of 1:1 dichloromethane/toluene and cooled to −78° C. Diisobutylaluminum hydride (1 M in hexanes, 0.36 mL) was added, and the mixture was stirred for 20 minutes. The reaction was quenched by the addition of water; the mixture was warmed to ambient temperature, and then acidified to pH˜2 by addition of concentrated HCl. The mixture was extracted with ethyl acetate; the organics were washed with brine and dried over Na2SO4. The solvents were removed in vacuo; the residue was purified by chromatography on an Analogix Intelliflash 280™, eluting with 17% ethyl acetate in hexanes to give the titled compound (25 mg, 68%).
후처리
- customThe reaction was quenched by the addition of water
- temperaturethe mixture was warmed to ambient temperature
- additionacidified to pH˜2 by addition of concentrated HCl
- extractionThe mixture was extracted with ethyl acetate
- washthe organics were washed with brine
- dry with materialdried over Na2SO4
- customThe solvents were removed in vacuo
- customthe residue was purified by chromatography on an Analogix Intelliflash 280™
- washeluting with 17% ethyl acetate in hexanes
출처 및 근거
- ORD 기록
- ord-7e5502f2a60548b8a139903ef04181b0
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08377913B2
연결된 노트
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