HRID45449

反应详情

EQUATION

反应方程式

HRID 45449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 12 (0.13 g, 0.31 mmol) in methanol (10 mL) and ethyl acetate (30 mL) was treated with 20% palladium on activated carbon (50% wet, 0.05 g) and was hydrogenated at 10 psi in a Parr shaker for 2 hr. The catalyst was filtered out and washed with ethyl acetate. The solvent was removed in a rotary evaporator and the crude product was purified by chromatography on silica (25 g) with 5% ethyl acetate in hexane (3 L). Pure B1 (0.08 g, 80%) was isolated.

WORKUP

后处理

  1. filtrationThe catalyst was filtered out
  2. washwashed with ethyl acetate
  3. customThe solvent was removed in a rotary evaporator
  4. customthe crude product was purified by chromatography on silica (25 g) with 5% ethyl acetate in hexane (3 L)