HRID219756

反应详情

EQUATION

反应方程式

HRID 219756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.3 g (10.6 mMol) of potassium tert-butanolate are added to 5.5 g (18.7 mMol) of the intermediate 1b in 40 ml of DMF at 0° C. The reaction mixture was stirred for 1 h. Then 4.25 g (18.7 mMol) of 8-quinolinesulfonyl chloride were added at 0° C. The reaction solution was stirred at 0° C. for three hours and then at room temperature for 16 h. This reaction solution was poured into aqueous K2CO3 solution, resulting in a precipitate which was isolated. This solid was dissolved in methylene chloride, dried and concentrated in vacuo. The resulting residue was recrystallized from ethanol. 6.2 g of the product were obtained.

WORKUP

后处理

  1. stirringThe reaction solution was stirred at 0° C. for three hours
  2. waitat room temperature for 16 h
  3. customresulting in a precipitate which
  4. customwas isolated
  5. customdried
  6. concentrationconcentrated in vacuo
  7. customThe resulting residue was recrystallized from ethanol