HRID45441

反应详情

EQUATION

反应方程式

HRID 45441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 5 (1.12 g, 2.67 mmol) in methanol (40 mL) and ethyl acetate (80 mL) was treated with 20% palladium on activated carbon (0.2 g, 0% wet) and hydrogenated in a Parr shaker at 10 psi for 3.5 hr. The catalyst was filtered off and washed with ethyl acetate. The solvent was removed on a rotary evaporator and the crude product was purified by chromatography on silica (80 g) with 2% ethyl acetate in hexane (1 L), then 4% (2 L) to yield pure A2 (0.75 g, 85%).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. washwashed with ethyl acetate
  3. customThe solvent was removed on a rotary evaporator
  4. customthe crude product was purified by chromatography on silica (80 g) with 2% ethyl acetate in hexane (1 L)