HRID1090104

反应详情

EQUATION

反应方程式

HRID 1090104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

16.95 cm3 of a 1.6M solution of n-butyllithium in n-hexane is added drop by drop to 2.29 g of 2-pyrrolidinone in solution in 160 cm3 of anhydrous tetrahydrofuran cooled to -30° C., maintaining the temperature at -30° C. After agitation for 30 minutes, the mixture is poured drop by drop into a solution containing 6 g of 4-methylthio-benzenesulphonyl chloride [J. Chem. Soc. (1948) 604] in 10 cm3 of tetrahydrofuran, operating between -30° and -25° C. The whole is left to return to ambient temperature. The solvent is evaporated off under reduced pressure, the residue is taken up in water and the solid is filtered off. After crystallization from isopropanol, 3.80 g of expected product is obtained.

WORKUP

后处理

  1. temperaturemaintaining the temperature at -30° C
  2. additionthe mixture is poured drop by drop into a solution
  3. customoperating between -30° and -25° C
  4. waitThe whole is left
  5. customto return to ambient temperature
  6. customThe solvent is evaporated off under reduced pressure
  7. filtrationthe solid is filtered off
  8. customAfter crystallization from isopropanol