Sodium hydride → Oxolan-2-yl 1-ethenyl-2-oxopyrrolidine-3-carboxylate
반응식
[C:1]([O:5][C:6]([CH:8]1[CH2:12][CH2:11][N:10]([CH:13]=[CH2:14])[C:9]1=[O:15])=[O:7])([CH3:4])(C)C.[H-].[Na+].Cl[CH:19]1[CH2:23]CC[O:20]1>O1CCCC1.C(OCC)C>[O:20]1[CH2:19][CH2:23][CH2:4][CH:1]1[O:5][C:6]([CH:8]1[CH2:12][CH2:11][N:10]([CH:13]=[CH2:14])[C:9]1=[O:15])=[O:7]참가 물질
6
실험 절차
8.9 g or 3-(t-butoxycarbonyl)-1-vinyl-2-pyrrolidinone (BCVP) was dissolved in 50 ml of tetrahydrofuran free of moisture. To this solution 1.0 g of sodium hydride and 4.4 g of 2-chlorotetrahydrofuran were added and allowed to react at room temperature for 1 hour. This solution was diluted with diethylether and washed many times with pure water. The organic solvent of the organic phase was evaporated and the residue was subjected to silica gel column chromatography, to obtain 9.3 g of pure 3-(tetrahydrofuranyloxycarbonyl)-1-vinyl-2-pyrrolidinone (hereinafter referred to as “TFVP”). Its chemical structure was determined by IR spectra and NMR.
후처리
- customto react at room temperature for 1 hour
- washwashed many times with pure water
- customThe organic solvent of the organic phase was evaporated
출처 및 근거
- ORD 기록
- ord-6fdd0a8cf79049a5b451472014cfbef5
- 출처 데이터셋
- uspto-grants-2001_07
- 특허 번호
- US06262222B1
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