HRID1248888
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
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
- temperatureThe reaction mixture is heated for five hours at the boil
- temperaturecooled
- filtrationThe resulting solid is filtered off
- customdried
- filtrationagain filtered off
- customAfter the solid thus obtained
- customhas been twice recrystallised from toluene, 743 g (31.8% of theory) of the desired pyrimidine, melting point 114° C.
- customare obtained