反应详情

49.7 g (0.253 mol) of 2-methyl-3-nitro-6-aminobenzoic acid are dissolved in 380 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 dropwise 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, and the mixture is subsequently refluxed for a further three hours and then allowed to cool. After pouring the reaction mixture into 1.8 l of water, it is extracted with methylene chloride. After drying the organic phase, it is concentrated. The solid obtained is sufficiently pure for the subsequent reaction (NMR).

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