反应详情

1.25 g (4.09 mmol) of 3-[4-(2-cyclopropylphenyl)piperazin-1-yl]-N-methylpropanamine, 150 ml of acetonitrile, 0.645 g (4.09 mmol) of 2-chloropyrimidine-4-carboxamide and 1 g of potassium carbonate are introduced into a 250-ml round bottom flask fitted with a condenser and with a calcium chloride safety tube. The mixture is heated under reflux for 6 h, is allowed to return to room temperature, is partially concentrated and water and dichloromethane are added. The organic phase is separated off, is washed with water and is dried over sodium sulphate, the solvent is evaporated off and the residue is purified by chromatography on a column of silica gel. The oily product obtained crystallises from acetonitrile and is separated off by filtration, is rinsed with diethyl ether and is dried while heated under vacuum. 0.97 g of compound are finally isolated.

1. customfitted with a condenser and with a calcium chloride safety tube
2. temperatureThe mixture is heated
3. temperatureunder reflux for 6 h
4. customto return to room temperature
5. concentrationis partially concentrated
6. additionwater and dichloromethane are added
7. customThe organic phase is separated off
8. washis washed with water
9. dry with materialis dried over sodium sulphate
10. customthe solvent is evaporated off
11. customthe residue is purified by chromatography on a column of silica gel
12. customThe oily product obtained
13. customcrystallises from acetonitrile
14. customis separated off by filtration
15. washis rinsed with diethyl ether
16. customis dried
17. temperaturewhile heated under vacuum