반응식
[Si]([O:8][C@H:9]1[C@H:23](/[CH:24]=[CH:25]/[C@@H:26]([OH:32])[CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C@@H:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[C:11](=[O:33])[CH2:10]1)(C(C)(C)C)(C)C.C(=O)([O-])[O-].[Na+].[Na+]>>[OH:8][C@H:9]1[C@H:23](/[CH:24]=[CH:25]/[C@@H:26]([OH:32])[CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C@@H:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[C:11](=[O:33])[CH2:10]1참가 물질
3
반응 조건
- 온도
- 40 °C
실험 절차
(−)-methyl(11R, 15S, 13E)-11-tert-butyldimethylsilyloxy-15-hydroxy-9-oxoprost-13-en-1-oate (481 mg, 1.0 mmol) was dissolved in 5 ml of a mixed solvent (ethyl acetate/water/tetrahydrofuran 6:3:1) and stirred at 40° C. for 2 h. The reaction mixture was poured into a saturated aqueous sodium carbonate cooled with ice and extracted with ethyl acetate (100 ml) two times. The combined organic layer was washed with a saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated in vacuo to remove solvent. The residue was purified by silica gel column chromatography [ethyl acetate/hexane (2/1)] to give 312 mg (85% yield) of prostaglandin E1 methyl ester;
후처리
- temperaturecooled with ice
- extractionextracted with ethyl acetate (100 ml) two times
- washThe combined organic layer was washed with a saturated aqueous sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- customto remove solvent
- customThe residue was purified by silica gel column chromatography [ethyl acetate/hexane (2/1)]
출처 및 근거
- ORD 기록
- ord-2b966432dd6d48f9b107f149ad16336b
- 출처 데이터셋
- uspto-grants-2001_11
- 특허 번호
- US06313341B1
연결된 노트
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