반응 #8715

반응 방정식

bromopropane

ethyl acetamidocyanoacetate

sodium

bromopropane

→

Ethyl 2-acetylamino-2-cyanopentanoate

용매

ethanol

ethanol

ethanol

반응 조건

후처리

1. 1
   기타After a clear solution has formed
2. 2
   온도the reaction mixture is heated
3. 3
   온도under reflux for 16 hours
4. 4
   기타The solvent is removed in vacuo
5. 5
   세척the solution is washed with water
6. 6
   건조dried over magnesium sulfate
7. 7
   기타The solvent is removed in vacuo
8. 8
   workup.STIRRINGthe residue is stirred up with petroleum ether
9. 9
   여과After filtering off with suction, 7.5 g (60%) of ethyl 2-acetylamino-2-cyanopentanoate
10. 10
    기타are obtained

실험 절차

1.35 g of sodium (58.8 mmol) are dissolved in 200 ml of ethanol and the resulting solution is cooled down to 0° C. 10 g (58.8 mmol) of ethyl acetamidocyanoacetate are added. After a clear solution has formed, a solution of 7.23 g (58.8 mmol) of bromopropane in 10 ml of ethanol is added dropwise and the reaction mixture is stirred at room temperature for 2 hours. A solution of 7.23 g (58.8 mmol) of bromopropane in 10 ml of ethanol is added once again and the reaction mixture is heated under reflux for 16 hours. The solvent is removed in vacuo and the residue is taken up in dichloromethane; the solution is washed with water and dried over magnesium sulfate. The solvent is removed in vacuo and the residue is stirred up with petroleum ether. After filtering off with suction, 7.5 g (60%) of ethyl 2-acetylamino-2-cyanopentanoate are obtained.

출처