HRID528752

反应详情

EQUATION

反应方程式

HRID 528752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 0.3 g (1.6 mmol) 3-hydroxymethyl-azetidine-1-carboxylic acid tert-butyl ester (route 15, step a) in 3 mL DCM at 0° C. were added 0.33 mL (2.4 mmol) triethylamine and 0.19 mL (2.4 mmol) methanesulfonyl chloride. The reaction was allowed to warm to room temperature and stirred for 3 hours. 10 mL DCM was added and the mixture was washed with H2O (3×15 mL). The organic phase was dried over Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, heptane/EtOAc 7:3 to 6:4).

WORKUP

后处理

  1. washthe mixture was washed with H2O (3×15 mL)
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationAfter filtration and evaporation of the solvent the product
  4. customwas purified by column chromatography (silica, heptane/EtOAc 7:3 to 6:4)