HRID553769

反应详情

EQUATION

反应方程式

HRID 553769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-Amino-5-(4-Methyl-2-oxo-2H-pyridin-1-yl)benzoic acid methyl ester (500 mg, 1.93 mmol) and NaN3 (233 g, 3.58 mmol) in AcOH was added HC(OEt)3 (1378.6 mg, 9.3 mmol) at room temperature. The reaction mixture was heated to reflux for 4 hours and then cooled to room temperature. The solvent was removed in vacuo and the residue was purified by silica-gel chromatography to give 3-(4-Methyl-2-oxo-2H-pyridin-1-yl)-5-tetrazol-1-yl-benzoic acid methyl ester as a light yellow solid (602 mg, 100%). MS (M+H)=312.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 hours
  3. customThe solvent was removed in vacuo
  4. customthe residue was purified by silica-gel chromatography