HRID255946

反应详情

EQUATION

反应方程式

HRID 255946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe mixture is then subsequently stirred at 0° C.
  2. additionpoured onto ice
  3. extractionextracted with diethyl ether
  4. customThe organic phase is separated off
  5. dry with materialdried with Na2SO4
  6. concentrationconcentrated in a rotary vacuum evaporator
  7. customThe light yellow residue is separated on a silica gel column (eluting agent: hexane/ethyl acetate 1:1)
  8. customWhite crystals of melting point 75°-77° C. then result