HRID218508

反应详情

EQUATION

反应方程式

HRID 218508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

30 g (128 mmol) of the compound from example 26A are dissolved in 1.3 l of anhydrous toluene and admixed with 45 g (192 mmol) of silver(I) oxide and 24.6 g (769 mmol) of anhydrous methanol. The mixture is heated to 60° C. for 16 h. It is then allowed to cool and filtered through silica gel. The product is fractionally eluted with a gradient of cyclohexane and 25:1 cyclohexane/ethyl acetate. The product fractions are concentrated to dryness under reduced pressure and dried under reduced pressure. This affords 17 g (72% of theory) of the desired product.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationfiltered through silica gel
  3. washThe product is fractionally eluted with a gradient of cyclohexane and 25:1 cyclohexane/ethyl acetate
  4. concentrationThe product fractions are concentrated to dryness under reduced pressure
  5. customdried under reduced pressure