Methyl Acrylate → (E)-3-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-acrylic acid methyl ester

温度

130 °C

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.

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

ORDレコード

ord-5ba138c63e8a414fbac0e1ce6a081e0d

出典データセット

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08748435B2