HRID41683

反应详情

EQUATION

反应方程式

HRID 41683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a suspension of 10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (9.97 g, 60 mmol) in methanol (200 ml) is added sodium tetrachloroaurate (597 mg, 1.5 mmol) and the reaction mixture is heated to 60° C. for 7 hours. The reaction mixture is allowed to cool down to room temperature and left to stand overnight. The reaction mixture is concentrated under reduced pressure, dissolved in ethyl acetate (200 ml) and washed with aqueous 2N sodium carbonate (100 ml), followed by saturated brine (100 ml). The organic layer is then dried over magnesium sulphate and concentrated under reduced pressure to give 5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (8.62 g)

WORKUP

后处理

  1. temperatureto cool down to room temperature
  2. waitleft
  3. concentrationThe reaction mixture is concentrated under reduced pressure
  4. dissolutiondissolved in ethyl acetate (200 ml)
  5. washwashed with aqueous 2N sodium carbonate (100 ml)
  6. dry with materialThe organic layer is then dried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure