HRID906399

反应详情

EQUATION

反应方程式

HRID 906399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of 6-bromoisoquinolin-1(2H)-one (Example 1b, 1.5 g) dissolved in NMP (15 mL) was treated with potassium carbonate (1.48 g) and (3-bromo-2,2-dimethylpropoxy)(tert-butyl)dimethylsilane (2.26 g) under nitrogen. The resulting mixture was stirred at 70° C. for 10 h (low conversion), heating was continued at 100° C. for 10 h. The reaction mixture was diluted with water (250 mL), and extracted with ethyl acetate (300 mL). The organic was dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified (SiO2 chromatography, elution with 20% diethyl ether in isohexane) to afford the subtitle compound (1.30 g) as an oil.

WORKUP

后处理

  1. temperatureheating
  2. waitwas continued at 100° C. for 10 h
  3. extractionextracted with ethyl acetate (300 mL)
  4. dry with materialThe organic was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto afford crude product
  8. customThe crude product was purified
  9. wash(SiO2 chromatography, elution with 20% diethyl ether in isohexane)