HRID643674

反应详情

EQUATION

反应方程式

HRID 643674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 3-(3-(2-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyridin-7-yl)-4-methylbenzoic acid (444 mg, 1.22 mmol) in 15 mL of THF at RT was added CDI (218 mg, 1.34 mmol). The resulting mixture was heated for 1 h at 50° C. The reaction mixture was then cooled to RT and tert-butyl carbazate (177 mg, 1.34 mmol) was added. The reaction mixture was again heated at 50° C. for 24 h. After the reaction mixture was concentrated to dryness, the residue was purified on the ISCO (40 g column, 50-100% EtOAc in Hexanes) to afford the title compound as an off-white amorphous solid. MS (ESI, pos. ion) m/z: 478.1 (M+1).

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to RT
  2. temperatureThe reaction mixture was again heated at 50° C. for 24 h
  3. concentrationAfter the reaction mixture was concentrated to dryness
  4. customthe residue was purified on the ISCO (40 g column, 50-100% EtOAc in Hexanes)