反应 #903
ord-24a3ddd0c4da4019a874af8b0e5c2e2d
反应方程式
反应物
试剂
反应条件
后处理
- 1温度The mixture is then heated
- 2其他thus obtained
- 3温度the mixture is subsequently refluxed for a further three hours
- 4温度to cool
- 5萃取is extracted with methylene chloride
- 6其他After drying the organic phase, it
- 7浓缩is concentrated
- 8其他The solid obtained
- 9其他is sufficiently pure for the subsequent reaction (NMR)
实验过程
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).