HRID81589

反应详情

EQUATION

反应方程式

HRID 81589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-(5-bromo-2-fluoro-phenyl)-5-hydroxymethyl-morpholin-3-one (1.6 g, 5.26 mmol) in 30 ml THF was added dropwise diethylaminosulfur trifluoride (0.97 ml, 7.34 mmol) and stirred for 2 h. The colorless solution was slowly added to an ice cooled Na2CO3 solution (10%, aqueous) and extracted with TBME. The organic layer was washed with brine, dried with MgSO4 and evaporated. The crude product was purified by chromatography on silica gel (heptane/EtOAc 3/1) to provide the title compound as a slightly yellow solid.

WORKUP

后处理

  1. extractionextracted with TBME
  2. washThe organic layer was washed with brine
  3. dry with materialdried with MgSO4
  4. customevaporated
  5. customThe crude product was purified by chromatography on silica gel (heptane/EtOAc 3/1)