反应 #1880972
ord-bc182c6d39aa465a81809ca9d164bfbf
反应方程式
DEAE
(R)-(+)-glycidol
phthalimide
triphenyl phosphine
→
desired product
收率 75.4%
N-(2(R), 3-Epoxypropyl)phthalimide
收率 75.4%
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度under cooling on ice-bath
- 2其他Molecular shieve was removed by filtration and filtrate
- 3其他was evaporated to dryness in vacuo
- 4其他The desired product was further purified by silica gel chromatography
实验过程
To THF solution (400 ml) of (R)-(+)-glycidol 2.47 g (32 mmol), phthalimide 7 g (47.6 mmol), triphenyl phosphine 14.3 g (54.5 mmol) and molecular shieve 4 Å 30 g were added at room temperature and then DEAE 8.7 g (50 mmol) was added dropwise under cooling on ice-bath. The reaction mixture was allowed to stand at room temperature overnight. Molecular shieve was removed by filtration and filtrate was evaporated to dryness in vacuo. The desired product was further purified by silica gel chromatography. 4.9 g of desired product was obtained as an oil. The NMR spectra were consistent with the desired title intermediate.