반응 #52186

반응 방정식

dimethyl sulphate

4-methylamino-3-nitro-benzoic acid

K2CO3

→

Methylamino-3-nitro-benzoic acid-methyl ester

용매

water

dimethyl formamide

반응 조건

후처리

1. 1
   workup.STIRRINGIt is stirred for 15 minutes
2. 2
   온도After cooling
3. 3
   여과the precipitated solids are filtered off
4. 4
   세척washed with water
5. 5
   기타dried

실험 절차

9.8 g (50 mmol) of 4-methylamino-3-nitro-benzoic acid are treated in 50 ml of dimethyl formamide (DMF) with K2CO3 (14 g). 5 ml of dimethyl sulphate are added dropwise to this mixture over 10 minutes with stirring. It is stirred for 15 minutes and heated for 0.5 hours at 60° C. After cooling, it is diluted with water, the precipitated solids are filtered off, washed with water and dried. Yield: 9.8 g (93%); M.Pt.: 138-140° C.

출처