HRID714808

反应详情

EQUATION

反应方程式

HRID 714808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 1-(2-chloropyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile (20 mg) obtained in Step A of Example 2 and 4-(aminomethyl)benzonitrile hydrochloride (27 mg) in N-methylpyrrolidone (2 mL) was added diisopropylethylamine (0.028 mL), and the mixture was stirred at 60° C. for 3 hr. To the reaction mixture were added ethyl acetate (3 mL) and water (1 mL), and the mixture was stirred for 5 min. The organic layer was filtered through Top-Phase Separation Filter Tube, and the solvent was evaporated at 60° C. The residue was purified by HPLC (C18, mobile phase: acetonitrile/10 mM aqueous ammonium hydrogen carbonate solution), and dried at 60° C. to give the title compound.

WORKUP

后处理

  1. stirringthe mixture was stirred for 5 min
  2. filtrationThe organic layer was filtered through Top-Phase Separation
  3. filtrationFilter Tube
  4. customthe solvent was evaporated at 60° C
  5. customThe residue was purified by HPLC (C18, mobile phase: acetonitrile/10 mM aqueous ammonium hydrogen carbonate solution)
  6. customdried at 60° C.