HRID70657

反应详情

EQUATION

反应方程式

HRID 70657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

Anisole (0.25 mL) was added to a solution of 6-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-3-ethylpyridin-2(1H)-one (49 mg) in trifluoroacetic acid (0.5 mL), and the mixture was stirred at 65° C. for seven hours. Trifluoroacetic acid (0.5 mL) was added and the mixture was stirred for further five hours, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1). The resulting crystals (25 mg) were recrystallized from ethyl acetate-hexane to give the title compound as a colorless powder (20 mg).

WORKUP

后处理

  1. stirringthe mixture was stirred for further five hours
  2. customafter which the solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1)
  4. customThe resulting crystals (25 mg) were recrystallized from ethyl acetate-hexane