반응 #903
ord-24a3ddd0c4da4019a874af8b0e5c2e2d
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반응물
시약
반응 조건
후처리
- 1온도The mixture is then heated
- 2기타thus obtained
- 3온도the mixture is subsequently refluxed for a further three hours
- 4온도to cool
- 5추출is extracted with methylene chloride
- 6기타After drying the organic phase, it
- 7농축is concentrated
- 8기타The solid obtained
- 9기타is sufficiently pure for the subsequent reaction (NMR)
실험 절차
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).