반응 #509013

반응 방정식

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

수율 4.5%

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

수율 4.5%

용매

ethanol

ethyl acetate

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도under reflux for 5 hours
3. 3
   기타the reaction liquid
4. 4
   기타was evaporated
5. 5
   workup.ADDITIONAcetic anhydride (3 mL) was added to the resulting residue
6. 6
   온도heated
7. 7
   온도under reflux for 2 hours
8. 8
   기타the reaction liquid
9. 9
   세척washed with water and saturated saline water
10. 10
    건조dried with anhydrous sodium sulfate
11. 11
    기타The solvent was evaporated away
12. 12
    기타the resulting residue was isolated
13. 13
    기타purified through thin-layer silica gel chromatography (chloroform/methanol=9/1)

실험 절차

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.

출처