HRID1010941

反应详情

EQUATION

反应方程式

HRID 1010941 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(tetrahydro-2H-pyran-3-yl)ethanol (1.54 gm) and triethylamine (3.3 ml) in dichloromethane (25 ml) was cooled (ice bath) and methanesulphonyl chloride (1.19 ml) added dropwise with stirring over 5 min. The reaction slowly warmed to ambient temperature as the ice bath melted. After 16 h the mixture was washed with saturated aq. sodium hydrogen carbonate, the aqueous layer extracted twice with dichloromethane and the combined extracts washed with dilute brine, dried by passing through a hydrophobic frit and evaporated to give the title compound as a brown oil, yield 2.38 g.

WORKUP

后处理

  1. additionadded dropwise
  2. customThe reaction
  3. washAfter 16 h the mixture was washed with saturated aq. sodium hydrogen carbonate
  4. extractionthe aqueous layer extracted twice with dichloromethane
  5. washthe combined extracts washed with dilute brine
  6. customdried
  7. customevaporated