Реакция #742891

Уравнение реакции

malonitrile

dimethylformamide

sodium hydride

5-(4-benzylpiperazin-1-yl)isatoic anhydride

→

2-Amino-3-cyano-4-hydroxy-6-(4-benzylpiperazin-1-yl)quinoline

Растворители

water

Условия реакции

Обработка

1. 1
   Экстракцияextracted with 2×50 mL of ethyl acetate
2. 2
   ДругоеThe aqueous phase is evaporated in vacuum
3. 3
   workup.DISSOLUTIONthe solid residue is dissolved in 50 mL of water
4. 4
   Температураrefluxed for 5 hours
5. 5
   ТемператураAfter cooling the precipitated material
6. 6
   Фильтрацияis filtered off
7. 7
   Промывкаwashed with water
8. 8
   СушкаAfter drying 14.3 g of the title compound
9. 9
   Другоеis obtained

Методика

6.1 g of malonitrile is dissolved in 100 mL of dimethylformamide. To the solution, in several portions, 3.6 g of 60% oily dispersion of sodium hydride are added. To the clear solution 18 g of 5-(4-benzylpiperazin-1-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction mixture is diluted with 100 mL of water and extracted with 2×50 mL of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 50 mL of water, the pH is adjusted to 6 with acetic acid and refluxed for 5 hours. After cooling the precipitated material is filtered off, washed with water. After drying 14.3 g of the title compound is obtained, m.p.: 291° C.

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