HRID420502

反应详情

EQUATION

反应方程式

HRID 420502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

In a sealed flask, a solution of 6-(2,4-dichloro-phenyl)-[1,2,4]triazolo[4,3-a]pyridine-7-carbonitrile (50 mg, 0.164 mmol) in THF (0.5 mL) was cooled to 0° C. (ice bath) then treated with BH3.THF complex (1.0 M solution in THF, 0.82 mL, 0.82 mmol). The reaction mixture was heated at 40° C. for 1 h, cooled to RT, and diluted in MeOH (large excess). The mixture was concentrated under vacuum, and the remaining residue was suspended in 2.0 M HCl, and shaken for 15 min. After evaporation to dryness, the remaining residue was purified by reverse phase prep-HPLC (Waters system) to give the title compound (2TFA salt, 1.9 mg, 0.004 mmol, 2%) as a white solid. MS: 293 [M+1]+; HPLC: AtRet=0.95.

WORKUP

后处理

  1. temperaturecooled to RT
  2. concentrationThe mixture was concentrated under vacuum
  3. customAfter evaporation to dryness
  4. customthe remaining residue was purified by reverse phase prep-HPLC (Waters system)