HRID403481
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThen the mixture was evaporated under reduced pressure
- additionThe residue was diluted with ethyl acetate
- washwashed with sat. NaHCO3— and NaCl-solution
- customdried over Na2 SO4
- customEvaporation
- customgave a yellow solid
- customThe crude product was purified by recrystallization from diethylether
- customto give a colorless solid