HRID874156

反应详情

EQUATION

反应方程式

HRID 874156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas then added dropwise
  2. filtrationAfter filtration
  3. washthe filter cake was washed with CH2Cl2
  4. washthe filtrate was washed twice with water
  5. customThe solvent was evaporated under vacuum
  6. customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate, 5:1)
  7. customto afford the target compound