HRID1919666
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
2-amino-3-bromobenzoic acid (1.00 g) was mixed with methanol (10 ml) and concentrated sulfuric acid (1 ml). The mixture was stirred at reflux for 31 hours. The solvent were evaporated, and saturated aqueous sodium bicarbonate was carefully added. The solid was extracted with CH2Cl2 (3×). The combined extracts were dried over Na2SO4 and the solvents removed in vacuo to afford methyl 2-amino-3-bromobenzoate as a semi-crystalline solid (976 mg, 91% yield). LCMS (ES): >85% pure, m/z 230 [M+1]+.
WORKUP
后处理
- temperatureat reflux for 31 hours
- customThe solvent were evaporated
- additionsaturated aqueous sodium bicarbonate was carefully added
- extractionThe solid was extracted with CH2Cl2 (3×)
- dry with materialThe combined extracts were dried over Na2SO4
- customthe solvents removed in vacuo