HRID49755

反应详情

EQUATION

反应方程式

HRID 49755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 9,10-dihydropyrrolo[2,1-b][1,3]benzothiazepin-9-one (0.24 g, 1.11 mmol), N-methylpiperazine (0.55 mL, 0.50 g, 4.99 mmol) and trimethylsilyl triflate (0.55 mL, 0.68 g, 3.05 mmol) was heated at 120° C. under stirring, after a few minutes further 0.55 mL of N-methylpiperazine were added and the reaction was kept for 3 hours at 120° C. After that time water was added and was extracted with dichloromethane. The organic layer was dried over sodium sulphate, filtered and evaporated to give the crude product that was purified by means of a flash chromatography (20% methanol in ethyl acetate) to afford 0.114 g of the pure title compound as a yellowish solid (84% yield).

WORKUP

后处理

  1. additionwere added
  2. extractionwas extracted with dichloromethane
  3. dry with materialThe organic layer was dried over sodium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. customto give the crude product that
  7. customwas purified by means of a flash chromatography (20% methanol in ethyl acetate)