HRID714779

反应详情

EQUATION

反应方程式

HRID 714779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-ethyl-1-(4-fluorobenzoyl)-2-oxopyrrolidine-3-carbonitrile (1.1 g) obtained in Step G in ethanol (15 mL) was added dropwise 28% aqueous ammonia solution (5 mL), and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate). The obtained crude crystals were dissolved in diisopropyl ether, and the remaining solid was removed by filtration. The solvent was evaporated under reduced pressure, and the resulting solid was collected by filtration, and washed with diisopropyl ether to give the title compound (82 mg).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)
  3. customThe obtained crude crystals
  4. customthe remaining solid was removed by filtration
  5. customThe solvent was evaporated under reduced pressure
  6. filtrationthe resulting solid was collected by filtration
  7. washwashed with diisopropyl ether