HRID1736000

反应详情

EQUATION

反应方程式

HRID 1736000 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 6-chloro-3,4-dihydro-4-hydroxy-2H-thieno[3,2-e]-1,2-thiazine 1,1-dioxide (2.0 g, 8.37 mmol) in DMF (50 mL) was added sodium hydride (0.37 g, 9.2 mmol), after stirring for 30 min 1,2-dibromoethane (2.36 g, 16.7 mmol) was added and this mixture was stirred at room temperature for 72 hr. The reaction mixture was poured into water and the aqueous mixture was extracted with ether. The combined extracts were dried (MgSO4) and evaporated to an oil which was purified by column chromatography (silica, 30% ethyl acetate/hexane) to give 1.52 g (53%) of the desired product as a viscous syrup which was used in the next step.

WORKUP

后处理

  1. additionwas added
  2. extractionthe aqueous mixture was extracted with ether
  3. dry with materialThe combined extracts were dried (MgSO4)
  4. customevaporated to an oil which
  5. customwas purified by column chromatography (silica, 30% ethyl acetate/hexane)