Piperazine → 1-(2-Pyrimidinyl)piperazine

A mixture of 3.2 g of 2-chloropyrimidine and 12.1 g of anhydrous piperazine in 100 ml of absolute ethanol is heated at reflux for 18 hours, then it is thoroughly evaporated under reduced pressure and in the warm. The residue is taken up with 400 ml of diethyl ether, the solution thus obtained is washed with 10 ml of an aqueous solution of sodium hydroxide 1:1, then with 20 ml of water. The organic solution is dried over anhydrous sodium sulfate, filtered and evaporated to dryness under reduced pressure. The oil thus obtained is dissolved in 30 ml of isopropanol and 4.38 g of 2-naphtalenesulfonic acid dissolved in 30 ml of isopropanol are added to the solution at about 60° C. From the solution thus obtained a product crystallizes which is filtered and dried to give 2-(1-piperazinyl)pyrimidine napsilate identical to the product of Example 1.

1. temperatureis heated
2. temperatureat reflux for 18 hours
3. customit is thoroughly evaporated under reduced pressure and in the warm
4. customthe solution thus obtained
5. washis washed with 10 ml of an aqueous solution of sodium hydroxide 1:1
6. dry with materialThe organic solution is dried over anhydrous sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness under reduced pressure
9. customThe oil thus obtained
10. additionare added to the solution at about 60° C
11. customFrom the solution thus obtained a product
12. customcrystallizes which
13. filtrationis filtered
14. customdried

ORD record

ord-106bd2fb67554ec3ab5adeb402279985

Source dataset

uspto-grants-1986_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04602015