반응식
C(=O)(O)[O-].[Na+].Cl[C:7]([O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:8].O1CCCC1.[F:22][C:23]1[CH:24]=[C:25]([C@H:31]2[NH:36][C@@H:35]([C@H:37]([OH:39])[CH3:38])[CH2:34][O:33][CH2:32]2)[CH:26]=[C:27]([F:30])[C:28]=1[F:29]>C(OCC)(=O)C.O>[CH2:10]([O:9][C:7]([N:36]1[C@H:31]([C:25]2[CH:24]=[C:23]([F:22])[C:28]([F:29])=[C:27]([F:30])[CH:26]=2)[CH2:32][O:33][CH2:34][C@@H:35]1[C@H:37]([OH:39])[CH3:38])=[O:8])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
Saturated sodium bicarbonate aqueous solution (20 mL) and benzyl chloroformate (1.31 mL) were added to a tetrahydrofuran (20 mL) solution of (R)-1-[(3R,5R)-5-(3,4,5-trifluorophenyl)morpholin-3-yl]ethanol (2 g). After stirring the reaction solution for 16 hours at room temperature, additional benzyl chloroformate (1.33 mL) was added, and the resultant was further stirred for 20 hours. Water and ethyl acetate were added, and the organic layer was partitioned. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was removed under a vacuum. The residue was purified by silica gel column chromatography (heptane/ethyl acetate), and the title compound (880 mg) was obtained. The physical property values are as follows.
후처리
- stirringthe resultant was further stirred for 20 hours
- customthe organic layer was partitioned
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was removed under a vacuum
- customThe residue was purified by silica gel column chromatography (heptane/ethyl acetate)
출처 및 근거
- ORD 기록
- ord-c0d90e89cdf742cb928f5520b1f6b064
- 출처 데이터셋
- uspto-grants-2011_08
- 특허 번호
- US08008293B2
연결된 노트
불러오는 중…