反应详情

温度

140 °C

A mixture of 36 g of 1-(4-methoxyphenyl)piperazine dihydrochloride, 22 g of 2-chloro-5-nitropyridine, 58 g of potassium carbonate and 227 ml of dimethyl sulfoxide was stirred overnight at 140° C. The reaction mixture was cooled and poured onto water. The precipitated product was filtered off, washed with water and dissolved in dichloromethane. The solution was treated with activated charcoal. The latter is filtered off and the filtrate was evaporated. The residue was triturated in 2-propanol. The product was filtered off and crystallized from 1-butanol, yielding 24.5 g of 1-(4-methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine; mp. 170° C. (interm. 21).

1. temperatureThe reaction mixture was cooled
2. additionpoured onto water
3. filtrationThe precipitated product was filtered off
4. washwashed with water
5. dissolutiondissolved in dichloromethane
6. additionThe solution was treated with activated charcoal
7. filtrationThe latter is filtered off
8. customthe filtrate was evaporated
9. customThe residue was triturated in 2-propanol
10. filtrationThe product was filtered off
11. customcrystallized from 1-butanol