HRID445927
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
PROCEDURE
实验过程
N-[5-bromomethyl-4-(4-fluorophenyl)-6-isopropyl-pyrimidin-2-yl]-N-methyl-methanesulfonamide (55.3 g) and toluene (500.0 mL) were added to a reactor. The reaction mixture was cooled to 0˜5° C. and then tributylphosphine (35.0 mL) was added thereto. The temperature of the reaction mixture was raised to 10˜20° C. The reaction mixture was stirred at the same temperature for 3 hours and then filtered under reduced pressure. The resulting white solid was washed with toluene (331.0 mL) and then dried under reduced pressure to obtain tributyl[2-(N-methyl-N-methanesulfonylamino)-4-(4-fluorophenyl)-6-isopropyl-pyrimidin-5-ylmethyl]phosphonium bromide as a white solid (80.1 g, yield 97.6%).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to 0˜5° C.
- temperatureThe temperature of the reaction mixture was raised to 10˜20° C
- filtrationfiltered under reduced pressure
- washThe resulting white solid was washed with toluene (331.0 mL)
- customdried under reduced pressure