HRID906435

反应详情

EQUATION

反应方程式

HRID 906435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of tert-butyl (2S)-4-{[6-bromo-1-oxo-2-(phenylsulfonyl)-1,2-dihydroisoquinolin-4-yl]methyl}-2-methylpiperazine-1-carboxylate (Example 34a, 3.2 g) dissolved in DMF (20 mL) was treated with sodium hydroxide (0.444 g) in water (20 mL) under nitrogen. The resulting mixture was stirred at 20° C. for 2 h. The reaction mixture was diluted with water (20 mL), and extracted with ethyl acetate (25 mL). The organics were dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified (SiO2 chromatography, elution 100% diethyl ether). Pure fractions were evaporated to dryness to afford the subtitle compound (0.780 g) as a solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (25 mL)
  2. dry with materialThe organics were dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customto afford crude product
  6. customThe crude product was purified
  7. wash(SiO2 chromatography, elution 100% diethyl ether)
  8. customPure fractions were evaporated to dryness