Reaktion #509013

Reaktionsgleichung

2,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)piperazine-1-carboxylate

2,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)-1-piperazinecarboxylate

hydrazine acetate

potassium carbonate

→

entitled compound

Ausbeute 4.5%

2,2-Dimethylpropyl 4-[4-(5-methyl-1,2,4-triazol-3-yl)pyridin-2-yl]-1-piperazinecarboxylate

Ausbeute 4.5%

Lösungsmittel

ethanol

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturunder reflux for 5 hours
3. 3
   Sonstigethe reaction liquid
4. 4
   Sonstigewas evaporated
5. 5
   workup.ADDITIONAcetic anhydride (3 mL) was added to the resulting residue
6. 6
   Temperaturheated
7. 7
   Temperaturunder reflux for 2 hours
8. 8
   Sonstigethe reaction liquid
9. 9
   Waschenwashed with water and saturated saline water
10. 10
    Trocknendried with anhydrous sodium sulfate
11. 11
    SonstigeThe solvent was evaporated away
12. 12
    Sonstigethe resulting residue was isolated
13. 13
    Sonstigepurified through thin-layer silica gel chromatography (chloroform/methanol=9/1)

Vorschrift

2,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)piperazine-1-carboxylate (143 mg) obtained in Example 2 was dissolved in ethanol (5 mL), and hydrazine acetate (140 mg) and potassium carbonate (328 mg) were added thereto and heated under reflux for 5 hours, then the reaction liquid was evaporated. Acetic anhydride (3 mL) was added to the resulting residue, and heated under reflux for 2 hours, then the reaction liquid was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was isolated and purified through thin-layer silica gel chromatography (chloroform/methanol=9/1) to obtain 7.6 mg of the entitled compound as a colorless oil.

Quelle