HRID714777

反应详情

EQUATION

反应方程式

HRID 714777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of N-(3-cyano-4,5-dihydrofuran-2-yl)-4-fluorobenzamide (5.0 g) obtained in Step E in N,N-dimethylformamide (30 mL) was added sodium iodide (6.5 g), and the mixture was stirred at 150° C. for 30 min. The solvent was evaporated under reduced pressure, and to the residue was added ice water. The resulting solid was collected by filtration, and washed with water. The residue was purified by silica gel column chromatography (hexane/ethyl acetate), and the resulting solid was washed with diisopropyl ether to give the title compound (1.3 g).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. additionto the residue was added ice water
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with water
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)
  6. washthe resulting solid was washed with diisopropyl ether