반응 #353244

반응 방정식

1-(4-methoxyphenyl)piperazine dihydrochloride

2-chloro-5-nitropyridine

potassium carbonate

→

1-(4-methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine

수율 57.4%

용매

dimethyl sulfoxide

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled
2. 2
   workup.ADDITIONpoured onto water
3. 3
   여과The precipitated product was filtered off
4. 4
   세척washed with water
5. 5
   workup.DISSOLUTIONdissolved in dichloromethane
6. 6
   workup.ADDITIONThe solution was treated with activated charcoal
7. 7
   여과The latter is filtered off
8. 8
   기타the filtrate was evaporated
9. 9
   기타The residue was triturated in 2-propanol
10. 10
    여과The product was filtered off
11. 11
    기타crystallized from 1-butanol

실험 절차

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).

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