HRID255946
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
7.5 g (30 mmol) of 2-[(4-tolylsulfonyl)oxy]-propionyl chloride are dissolved in 15 ml of tetrahydrofuran in a flask. 6.5 g (80 mmol) of morpholine are then slowly added dropwise at 0°-5° C., with stirring and simultaneous cooling. The mixture is then subsequently stirred at 0° C., poured onto ice and extracted with diethyl ether. The organic phase is separated off, dried with Na2SO4 and concentrated in a rotary vacuum evaporator. The light yellow residue is separated on a silica gel column (eluting agent: hexane/ethyl acetate 1:1). White crystals of melting point 75°-77° C. then result.
WORKUP
后处理
- stirringThe mixture is then subsequently stirred at 0° C.
- additionpoured onto ice
- extractionextracted with diethyl ether
- customThe organic phase is separated off
- dry with materialdried with Na2SO4
- concentrationconcentrated in a rotary vacuum evaporator
- customThe light yellow residue is separated on a silica gel column (eluting agent: hexane/ethyl acetate 1:1)
- customWhite crystals of melting point 75°-77° C. then result