HRID445927

反应详情

EQUATION

反应方程式

HRID 445927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was cooled to 0˜5° C.
  2. temperatureThe temperature of the reaction mixture was raised to 10˜20° C
  3. filtrationfiltered under reduced pressure
  4. washThe resulting white solid was washed with toluene (331.0 mL)
  5. customdried under reduced pressure