반응식
[F:1][C:2]([F:22])([F:21])[S:3]([NH:6][C:7]1[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][CH2:13][O:12][C:11]1=[O:16])(=[O:5])=[O:4].C(=O)([O-])O.[Na+].Cl[C:29]([O:31][CH2:32][CH2:33][CH3:34])=[O:30].O>C(#N)C>[CH2:32]([O:31][C:29]([N:6]([C:7]1[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][CH2:13][O:12][C:11]1=[O:16])[S:3]([C:2]([F:1])([F:21])[F:22])(=[O:5])=[O:4])=[O:30])[CH2:33][CH3:34]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one (0.13 g, 0.38 mmol) and sodium hydrogen carbonate (0.06 g, 0.71 mmol) was suspended in acetonitrile (15 ml), added with propyl chloroformate (0.09 g, 0.77 mmol) and heated to reflux for six hours. After cooling to room temperature, the reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4) to obtain 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one (0.11 g).
후처리
- temperatureheated
- temperatureto reflux for six hours
- extractionextracted with ethyl acetate
- washThe organic layer was washed with a saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)
출처 및 근거
- ORD 기록
- ord-6b8d7d689bc74860aaa9e3e40448eaac
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08048825B2
연결된 노트
불러오는 중…