HRID874156
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
At 0° C., to a solution of 2-(3-oxetanyl)ethanol (according to the synthesis procedure in the reference: Journal of American Chemical Society, 2009, 131, 2786-2787.) (193 mg, 1.89 mmol) in CH2Cl2 (15 mL) was added DABCO (847 mg, 7.56 mmol) and TsCl (1.43 g, 7.56 mmol) was then added dropwise, the mixture was stirred for 15 minutes. After filtration, the filter cake was washed with CH2Cl2 and the filtrate was washed twice with water. The organic phase was dries over anhydrous sodium sulphate. The solvent was evaporated under vacuum. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate, 5:1) to afford the target compound.
WORKUP
后处理
- additionwas then added dropwise
- filtrationAfter filtration
- washthe filter cake was washed with CH2Cl2
- washthe filtrate was washed twice with water
- customThe solvent was evaporated under vacuum
- customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate, 5:1)
- customto afford the target compound