HRID403481

反应详情

EQUATION

反应方程式

HRID 403481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

3-(4-Bromo-benzyl)-2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidine (3) (525 mg, 1.47 mmol) was dissolved in 15 ml of dioxane and after addition of methyl acrylate (264 ul, 2.93 mmol), dicyclohexyl-methylamine (622 ul ml, 2.93 mmol) and Pd(PtBu3)2 (15 mg, 0.03 mmol) the mixture was heated for 5 min at 130° C. in a microwave oven. Then the mixture was evaporated under reduced pressure. The residue was diluted with ethyl acetate, washed with sat. NaHCO3— and NaCl-solution, and dried over Na2 SO4. Evaporation gave a yellow solid. The crude product was purified by recrystallization from diethylether to give a colorless solid.

WORKUP

后处理

  1. customThen the mixture was evaporated under reduced pressure
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with sat. NaHCO3— and NaCl-solution
  4. customdried over Na2 SO4
  5. customEvaporation
  6. customgave a yellow solid
  7. customThe crude product was purified by recrystallization from diethylether
  8. customto give a colorless solid