HRID1051428

反应详情

EQUATION

反应方程式

HRID 1051428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customAfter POCl3 was evaporated
  2. customthe residue was quenched with ice water very carefully
  3. extractionextracted with ethyl acetate (3×30 mL)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated
  6. custompurified by prep-HPLC