HRID1930076
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe crude mixture was partitioned between water and DCM
- dry with materialThe organics were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto give a yellow solid
- customthat was triturated with Et2O
- filtrationfiltered