HRID456607

反应详情

EQUATION

反应方程式

HRID 456607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A solution of (a) (2 g, 8.7 mmol) in water (220 ml) containing sodium hydroxide (17 mmol) was hydrogenated over 10% palladium on charcoal (1g) for 4 hours. The mixture was filtered and evaporated to give a white solid. This solid was dissolved in N,N-dimethylformamide (8 ml) then treated with potassium carbonate (2.9 g) and 1,2-dibromoethane (0.6 ml, 7 mmol). The mixture was heated at 85° C. overnight. The cooled mixture was evaporated onto silica and chromatographed eluting with 10–30% methanol in ethyl acetate affording a white solid (250 mg, 21%).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customevaporated
  3. customto give a white solid
  4. customThe cooled mixture was evaporated onto silica
  5. customchromatographed
  6. washeluting with 10–30% methanol in ethyl acetate affording a white solid (250 mg, 21%)