HRID1249114
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
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 chloride-ethyl acetate. 3.4 g of product with m.p. 144°-145° C. is obtained.
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureto reflux for two hours
- customThe dimethylformamide is removed on a rotary evaporator
- customThe concentrated reaction mixture
- extractionThe crude product is extracted with CH2Cl2
- dry with materialThe crude extracts are dried with MgSO4
- filtrationfiltered
- concentrationconcentrated on a rotary evaporator
- customThe crude product is purified by recrystallization from butyl chloride-ethyl acetate