HRID868315
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Three hundred milligrams of the compound (VII) obtained in the above procedure (1) were dissolved in 80% trifluoroacetic acid solution and the resulting mixture was stirred at room temperature for 2 hours under a nitrogen gas stream. The reaction mixture was concentrated to dryness and the residue was purified by column chromatography on silica gel (10 g). A colorless oily substance was obtained from a 98:2 eluate of chloroform and methanol. The oily substance was crystallized from a mixed solvent of ethanol and petroleum ether to obtain 170 mg of the title compound as colorless needle-like crystals.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated to dryness
- customthe residue was purified by column chromatography on silica gel (10 g)
- customA colorless oily substance was obtained from a 98:2 eluate of chloroform and methanol
- customThe oily substance was crystallized from a mixed solvent of ethanol and petroleum ether