HRID720144

反应详情

EQUATION

反应方程式

HRID 720144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Palladium (10% on activated carbon) (0.23 g, 0.198 mmol) was added to a solution of the title compound of Example 164 (0.65 g, 1.99 mmol) in 1:10 N,N-dimethylformamide:methanol (11 mL). The reaction mixture was purged with H2 and stirred at room temperature under H2 (1 atm.) for 5 hours. The palladium was filtered and the volatile components were removed in vacuo. The resulting residue was dissolved in methanol and loaded onto a silica gel plug. The plug was then loaded onto a silica gel column and eluted with 1.2:1 dichloromethane:ethyl acetate to afford the title compound (0.45 g, 1.37 mmol) as a yellow solid in 69% yield.

WORKUP

后处理

  1. customThe reaction mixture was purged with H2
  2. filtrationThe palladium was filtered
  3. customthe volatile components were removed in vacuo
  4. dissolutionThe resulting residue was dissolved in methanol
  5. washeluted with 1.2:1 dichloromethane