HRID887824

反应详情

EQUATION

反应方程式

HRID 887824 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-[2-(5-chloro-2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethyl]acetamide (79.5 mg, 0.274 mmol) in tetrahydrofuran (5 mL) was added 5% platinum-activated carbon (32 mg), and the mixture was stirred under a hydrogen atmosphere at room temperature for 7 hr. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→25/75), liquid chromatography (water/acetonitrile=90/10→0/100) and recrystallization (ethyl acetate/hexane) to give the title compound (23.3 mg, yield 29%).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→25/75), liquid chromatography (water/acetonitrile=90/10→0/100) and recrystallization (ethyl acetate/hexane)