HRID484951

反应详情

EQUATION

反应方程式

HRID 484951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3.2 g of N-methyl methanesulfonamide in 50 ml of dry dimethylformamide is added 1.47 g of potassium methoxide. The mixture is stirred for 15 minutes. 2.8 g of 2-Fluoronitrobenzene is added and the mixture is heated to reflux for two hours. The dimethylformamide is removed on a rotary evaporator. The concentrated reaction mixture is poured into water. The crude product is extracted with CH2Cl2. The crude extracts are dried with MgSO4, filtered and concentrated on a rotary evaporator. The crude product is purified by recrystallization from butyl chlorideethyl acetate. 3.4 g of product with m.p. 144°-145° C. is obtained.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureto reflux for two hours
  3. customThe dimethylformamide is removed on a rotary evaporator
  4. customThe concentrated reaction mixture
  5. extractionThe crude product is extracted with CH2Cl2
  6. dry with materialThe crude extracts are dried with MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated on a rotary evaporator
  9. customThe crude product is purified by recrystallization from butyl chlorideethyl acetate