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
- 120 °C
PROCEDURE
实验过程
A microwave vial was charged with Mo(CO)6 (264 mg, 1.0 mmol), Herrmann's palladacycle (23 mg, 0.025 mmol), [(t-Bu)3PH]BF4 (15 mg, 0.050 mmol), 2-amino-6-bromo-8-(trans-4-hydroxycyclohexyl)-4-methylpyrido[2,3-d]pyrimidin-7(8H)-one (353 mg, 1.0 mmol), DMF (5 mL) and butanol (5 mL). DBU (412 ml, 3.0 mmol) was added, followed by rapid sealing of the vial under air. The vial was then heated to 120° C. by microwave irradiation for 30 minutes. After cooling, the reaction mixture was slurried with water and filtered. The precipitate was washed with ether and dried to afford 253 mg of butyl 2-amino-8-(trans-4-hydroxycyclohexyl)-4-methyl-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidine-6-carboxylate.
WORKUP
后处理
- temperatureAfter cooling
- filtrationfiltered
- washThe precipitate was washed with ether
- customdried