HRID1891044

反应详情

EQUATION

反应方程式

HRID 1891044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

248 mg of mCPBA was added to a 3:1 toluene-tetrahydrofuran (30 mL) solution containing 130 mg of 4-(methylamino)-2-(methylsulfanyl)pyrimidine-5-carbonitrile, and the mixture was stirred at room temperature for 15 minutes. Then, 138 mg of 4-(4-methylpiperazin-1-yl)aniline, and 280 mg of DIPEA were added to the mixture, which was then stirred at 80° C. for 8 hours. The solvent was distilled away after cooling the reaction mixture. Then, water was added, and the solution was extracted with ethyl acetate. The organic layer was washed with saturated saline, and the solution was concentrated after drying with anhydrous magnesium sulfate. The resulting crude product was purified by basic silica gel column chromatography, and 170 mg of a white solid was obtained as a subject compound.

WORKUP

后处理

  1. stirringwas then stirred at 80° C. for 8 hours
  2. distillationThe solvent was distilled away
  3. temperatureafter cooling the reaction mixture
  4. additionThen, water was added
  5. extractionthe solution was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated saline
  7. concentrationthe solution was concentrated
  8. dry with materialafter drying with anhydrous magnesium sulfate
  9. customThe resulting crude product was purified by basic silica gel column chromatography