HRID1930076

反应详情

EQUATION

反应方程式

HRID 1930076 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 6-(2,4-difluorophenyl)-5-(6-hydrazinylpyridazin-3-yl)imidazo[2,1-b]oxazole (0.300 g, 0.914 mmol, Example #40, Step B, was dissolved in MeOH (15 mL) at about ambient temperature before addition of Na2CO3 (0.112 g, 1.371 mmol). Cyanogen bromide (3M in DCM, 0.305 mL, 0.914 mmol) was added and the resulting mixture was stirred at about ambient temperature for about 1 h. The crude mixture was partitioned between water and DCM. The organics were dried over MgSO4, filtered, concentrated under reduced pressure to give a yellow solid that was triturated with Et2O and filtered to give the title compound (0.185 g, 57%): LC/MS (Table 1, Method g) Rt=1.65 min.; MS m/z: 354.07 (M+H)+.

WORKUP

后处理

  1. customThe crude mixture was partitioned between water and DCM
  2. dry with materialThe organics were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customto give a yellow solid
  6. customthat was triturated with Et2O
  7. filtrationfiltered