HRID391734

反应详情

EQUATION

反应方程式

HRID 391734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At 0° C., 37 g (49 mmol) of the compound from Example 24A are dissolved in 313 ml of 1.25N hydrochloric acid in methanol. After 1 h, the solution is evaporated under reduced pressure and diluted with dichloromethane. The organic phase is washed twice with water, dried over magnesium sulphate and, after filtration, evaporated to dryness under reduced pressure. The residue is chromatographed on silica gel using a gradient of dichloromethane and methanol. The product fractions are combined and evaporated to dryness under reduced pressure. This gives 19 g (78% of theory) of the desired product.

WORKUP

后处理

  1. customthe solution is evaporated under reduced pressure
  2. additiondiluted with dichloromethane
  3. washThe organic phase is washed twice with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationafter filtration
  6. customevaporated to dryness under reduced pressure
  7. customThe residue is chromatographed on silica gel using a gradient of dichloromethane and methanol
  8. customevaporated to dryness under reduced pressure