参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 二氧化碳 | HCID 280 | — |
| 反应物 | 甲基硫酸酯-13C2 | HCID 6497 | — |
| 反应物 | 碳酸氢钠 | HCID 516892 | — |
| 反应物 | 钠 | HCID 5360545 | — |
| 反应物 | 6-氨基-2-甲基-3-硝基苯甲酸 | HCID 15283172 | — |
| 溶剂 | 丙酮 | HCID 180 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | Methyl 6-amino-2-methyl-3-nitrobenzoate | HCID 15334532 | — |
反应步骤
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).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05723415 |
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| 来源数据集 | uspto-grants-1998_03 |
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| ORD ID | ord-24a3ddd0c4da4019a874af8b0e5c2e2d |
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| 来源说明 | uspto-grants-1998_03 |
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