反应详情

温度

30 °C

1-(2-hydroxyethyl)piperazine (Compound 3) (16.6 g, 127.6 mmol)) and 2-methyl-4,6-dichloropyrimidine (Compound 2) (10.4 g, 63.8 mmol) were mixed with methylene dichloride (80 mL) in reaction flask to be stirred for 2.5 h at 30° C., and then triethylamine (1.8 mL) was added with the reaction overnight in thermal insulation. After vacuum filtration, the cake was rinsed by methylene dichloride. The filtrate was vacuum condensed to dry, and then n-hexane (40 mL) was added to grow the grains for 1 h by stirring. After vacuum filtration, the cake was rinsed by n-hexane (20 mL) and dried at 40° C. to constant weight to give white solid target Compound 4 (14.7 g, yield: 89.8%).

1. filtrationAfter vacuum filtration
2. washthe cake was rinsed by methylene dichloride
3. customvacuum condensed
4. customto dry
5. additionn-hexane (40 mL) was added
6. customfor 1 h
7. stirringby stirring
8. filtrationAfter vacuum filtration
9. washthe cake was rinsed by n-hexane (20 mL)
10. customdried at 40° C. to constant weight