HRID1248888

反应详情

EQUATION

反应方程式

HRID 1248888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,850 g (9.31 moles) of 4-amino-2,5,6-trichloropyrimidine are dissolved in 4 liters of tetrahydrofuran. 1,659 g (18.62 moles) of 3-methoxypropylamine are added dropwise thereto over a period of 6 hours. The reaction mixture is heated for five hours at the boil, cooled and stirred into 20 liters of water. The resulting solid is filtered off, dried, stirred with 7 liters of methylene chloride and again filtered off. After the solid thus obtained has been twice recrystallised from toluene, 743 g (31.8% of theory) of the desired pyrimidine, melting point 114° C., are obtained.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated for five hours at the boil
  2. temperaturecooled
  3. filtrationThe resulting solid is filtered off
  4. customdried
  5. filtrationagain filtered off
  6. customAfter the solid thus obtained
  7. customhas been twice recrystallised from toluene, 743 g (31.8% of theory) of the desired pyrimidine, melting point 114° C.
  8. customare obtained