HRID1109565

反应详情

EQUATION

反应方程式

HRID 1109565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.96 ml of N,N-dimethylformamide di-t-butyl acetal was added dropwise within 20 minutes to a boiling solution of 0.34 g of 4,5-dihydro-7-oxo-8-(m-fluorophenyl)-7H-thieno[2,3-a]quinolizine-10-carboxylic acid in 5 ml of toluene. The mixture was heated under reflux for an additional 30 minutes, left to stand at room temperature overnight and then washed once with water, twice with saturated aqueous sodium bicarbonate solution and once with saturated aqueous sodium chloride solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The residue was recrystallized from ethyl acetate and there was obtained tert-butyl 8-(m-fluorophenyl)-4,5-dihydro-7-oxo-7H-thieno[2,3-a ]quinolizine-10-carboxylate of m.p. 135°-137°.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for an additional 30 minutes
  3. waitleft
  4. washwashed once with water, twice with saturated aqueous sodium bicarbonate solution and once with saturated aqueous sodium chloride solution
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. customevaporated in vacuo
  7. customThe residue was recrystallized from ethyl acetate