HRID1919666

反应详情

EQUATION

反应方程式

HRID 1919666 的结构方程式

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

  1. temperatureat reflux for 31 hours
  2. customThe solvent were evaporated
  3. additionsaturated aqueous sodium bicarbonate was carefully added
  4. extractionThe solid was extracted with CH2Cl2 (3×)
  5. dry with materialThe combined extracts were dried over Na2SO4
  6. customthe solvents removed in vacuo