HRID1297588

反应详情

EQUATION

反应方程式

HRID 1297588 的结构方程式

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To N-[4-(1-Carbamoyl-1-methyl-ethyl)-2-fluoro-benzyl]-2-(4-fluoro-phenoxy)-nicotinamide (3.00 g) in a 50 mL flask was added phosphorous oxychloride (3.29 mL). The solution was heated for 1 h at 90° C. The solution was then cooled in an ice bath, poured over satd. aq. sodium carbonate (50 mL), then extracted with ethyl acetate (4×100 mL). The combined organic layers were dried over magnesium sulfate, filtered, and concentrated in vacuo, yielding the title compound (2.36 g).

WORKUP

后处理

  1. temperatureThe solution was then cooled in an ice bath
  2. additionpoured over satd
  3. extractionaq. sodium carbonate (50 mL), then extracted with ethyl acetate (4×100 mL)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo