HRID887824
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- 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)