HRID1736356

反应详情

EQUATION

反应方程式

HRID 1736356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude ester (10 g, 38 mM) was dissolved in ethanol (20 ml) and added to a stirred suspension of SnCl2.2H2O (42.9 g, 0.19M) in ethanol (60 ml) under argon at ambient temperature. The mixture was heated to reflux for 30 minutes, cooled and poured onto ice. After making basic to pH 8 with an aqueous solution of sodium bicarbonate, the mixture was extracted with ethyl acetate. The combined extracts were washed with water and brine, dried over MgSO4 and evaporated to give allyl 3-allyloxy-4-aminobenzoate (8.2 g).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 30 minutes
  3. temperaturecooled
  4. additionpoured onto ice
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe combined extracts were washed with water and brine
  7. dry with materialdried over MgSO4
  8. customevaporated