HRID1930062

反应详情

EQUATION

反应方程式

HRID 1930062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

The 4-(4-(2,4-difluorophenyl)-5-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)thiazol-2-yl)cyclohexanone (0.495 g, 1.09 mmol, Example #26, Step B) was dissolved in MeOH (5 mL) then cooled to about −5° C. Sodium borohydride (0.0413 g, 1.09 mmol) was added and the mixture was stirred for about 5 min. Acetone was added then the solvents were concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel with DCM/MeOH (95:5) as an eluent then by RP-HPLC (Table 1, Method f) to give the title compound: (0.029 g, 6%): LC/MS (Table 1, Method a) Rt=2.41 min; MS m/z: 456.2 (M+H)+.

WORKUP

后处理

  1. concentrationthe solvents were concentrated under reduced pressure
  2. customthe residue was purified by flash chromatography on silica gel with DCM/MeOH (95:5) as an eluent