HRID1713542
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To 1,1-bis(phenylmethyl)-hexahydro-3H-oxazolo[3,4-a]pyrazin-3-one (0.16 g, 0.50 mmol) were added tetrahydrofuran (10 mL) and 4-fluorobenzyl isocyanate (0.30 g, 2.0 mmol), and the mixture was stirred at 50° C. for 4 hours. The reaction solution was concentrated, and then the residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate). The fractions were collected and concentrated. To the residue was added diisopropyl ether, and the obtained solid matter was collected by filtration and washed with diisopropyl ether to obtain the title compound (0.17 g, yield 70%).
WORKUP
后处理
- concentrationThe reaction solution was concentrated
- customthe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate)
- customThe fractions were collected
- concentrationconcentrated
- additionTo the residue was added diisopropyl ether
- filtrationthe obtained solid matter was collected by filtration
- washwashed with diisopropyl ether