HRID1850310

反应详情

EQUATION

反应方程式

HRID 1850310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-[3-(2-Hydroxy-ethyl)-oxetan-3-yl]-ethanol (123) (1.3 g, 8.9 mmol) in CH2Cl2 (20 mL) at 0° C. was added Et3N (2.7 g, 26.7 mmol) and methanesulfonyl chloride (2.0 g, 17.8 mmol). The solution was allowed to warm to RT and stirred for 15 min. The reaction mixture was diluted with water (80 mL). The aqueous phase was extracted with CH2Cl2 (3×50 mL) and the combined organic extracts were washed with brine (100 mL), dried over MgSO4, filtered, and concentrated to give the product (124) (2.0 g, 6.6 mmol, yield: 74%). ESI-MS (M+1): 303 calc. for C9H18O7S2 302.

WORKUP

后处理

  1. extractionThe aqueous phase was extracted with CH2Cl2 (3×50 mL)
  2. washthe combined organic extracts were washed with brine (100 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated