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
To a solution of hexahydro-1,1-diphenyl-3H-oxazolo[3,4-a]pyrazin-3-one (0.15 g, 0.50 mmol) in tetrahydrofuran (10 mL) were added triethylamine (0.14 mL, 1.0 mmol) and succinic anhydride (55 mg, 0.55 mmol), and the mixture was stirred at room temperature for 2 hours. To the reaction solution was added ethyl acetate, and the resulting mixture was washed with 2 M hydrochloric acid, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate). The fractions were concentrated, and to the residue was added diethyl ether. The resulting crystals were collected by filtration and washed with diethyl ether to obtain the title compound (99 mg, yield 50%).
WORKUP
后处理
- washthe resulting mixture was washed with 2 M hydrochloric acid
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate)
- concentrationThe fractions were concentrated
- additionto the residue was added diethyl ether
- filtrationThe resulting crystals were collected by filtration
- washwashed with diethyl ether