HRID657172

反应详情

EQUATION

反应方程式

HRID 657172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a round bottom flask was added 2-[(E)-2-phenylethenyl]-5,8-dihydropyrido[2,3-d]pyrimidin-7(6H)-one (600 mg, 2.39 mmol) in DMF (10 mL) and methanol (10 mL). Ozone was bubbled through the solution at room temperature for 20 minutes and the excess ozone was purged with a stream of nitrogen. Dimethyl sulfide (1.77 mL, 23.9 mmol) was added and the reaction was stirred at room temperature for 24 h. The solvent was evaporated and the resulting solid was dissolved in 20% MeOH-DCM. The crude product was added to a silica gel column and was eluted with 0-20% MeOH-DCM. The collected fractions gave the title compound (400 mg, 95% yield).

WORKUP

后处理

  1. customOzone was bubbled through the solution at room temperature for 20 minutes
  2. customthe excess ozone was purged with a stream of nitrogen
  3. customThe solvent was evaporated
  4. dissolutionthe resulting solid was dissolved in 20% MeOH-DCM
  5. additionThe crude product was added to a silica gel column
  6. washwas eluted with 0-20% MeOH-DCM