反应详情

49.7 g (0.253 mol) of 2-methyl-3-nitro-6-aminobenzoic acid are dissolved in380 ml of acetone and 43 g (0.51 mol) of sodium hydrogen carbonate are added. The mixture is then heated to boiling until evolution of CO2 is complete. 35.3 g (0.28 mol) of dimethyl sulfate are then added in the course of two hours at the boiling point of acetone to the suspension of the sodium salt of 2-methyl-3-nitro-6-aminobenzoic acid thus obtained, andthe mixture is subsequently refluxed for a further 3 hours and then allowedto cool. After pouring the reaction mixture into 1.8 l of water, it is extracted with methylene chloride. After drying, the organic phase is concentrated. The solid obtained is sufficiently pure for the subsequent reaction (NMR). Yield: 50 g (0.238 mol)=94% of theory, m.p.: 92°-94° C.

1. additionare added
2. temperatureThe mixture is then heated
3. customthus obtained
4. temperatureandthe mixture is subsequently refluxed for a further 3 hours
5. extractionis extracted with methylene chloride
6. customAfter drying
7. concentrationthe organic phase is concentrated
8. customThe solid obtained
9. customis sufficiently pure for the subsequent reaction (NMR)