HRID510034

反应详情

EQUATION

反应方程式

HRID 510034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

39.23 g (85.75 mmol) of the compound from example 29A were initially charged in DMF (800 ml) and then 4 g of palladium (10% on charcoal) were added. Hydrogenation was effected at standard hydrogen pressure while stirring overnight. The mixture was filtered through kieselguhr, washed through with a little DMF and a little methanol and concentrated to dryness. The residue was admixed with ethyl acetate and stirred vigorously, and the precipitate was filtered off with suction, washed with ethyl acetate and diisopropyl ether and dried under a high vacuum over Sicapent.

WORKUP

后处理

  1. filtrationThe mixture was filtered through kieselguhr
  2. washwashed through with a little DMF
  3. concentrationa little methanol and concentrated to dryness
  4. stirringstirred vigorously
  5. filtrationthe precipitate was filtered off with suction
  6. washwashed with ethyl acetate and diisopropyl ether
  7. customdried under a high vacuum over Sicapent