HRID2036604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
The crude 2-(cyclopropylamino)-3-nitrobenzoic acid (0.90 g, 4.1 mmol) was dissolved in MeOH (15 mL), and 2 mL H2SO4 (98%) was added. The mixture was heated to reflux for 18 h. The mixture was cooled, concentrated in vacuo, and purified by column chromatography on a silica gel column using DCM as eluent to give methyl 2-(cyclopropylamino)-3-nitrobenzoate: LC-MS (ESI) m/z 237.1 [M+H]+.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 18 h
- temperatureThe mixture was cooled
- concentrationconcentrated in vacuo
- custompurified by column chromatography on a silica gel column