HRID1051428
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
N-(2-methyl-4-(4-methyl-2-propyl-1H-imidazol-1-yl)thiazol-5-yl)acetamide (60 mg, 0.2 mmol) was suspended in phosphorus oxychloride (5 mL) and P2O5 (280 mg, 2 mmol) was added quickly. The resulting mixture was heated at 130° C. in a sealed tube overnight. After POCl3 was evaporated, the residue was quenched with ice water very carefully. The mixture was neutralized with saturated Na2CO3 solution and extracted with ethyl acetate (3×30 mL). The organic layer was dried over Na2SO4, concentrated and purified by prep-HPLC to give 4 mg of the title compound.
WORKUP
后处理
- customAfter POCl3 was evaporated
- customthe residue was quenched with ice water very carefully
- extractionextracted with ethyl acetate (3×30 mL)
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated
- custompurified by prep-HPLC