تفاعل #8715

ord-62e21300892c4773a62144aa95cd1bda

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter a clear solution has formed
  2. 2
    درجة الحرارةthe reaction mixture is heated
  3. 3
    درجة الحرارةunder reflux for 16 hours
  4. 4
    أخرىThe solvent is removed in vacuo
  5. 5
    غسيلthe solution is washed with water
  6. 6
    تجفيفdried over magnesium sulfate
  7. 7
    أخرىThe solvent is removed in vacuo
  8. 8
    workup.STIRRINGthe residue is stirred up with petroleum ether
  9. 9
    ترشيحAfter filtering off with suction, 7.5 g (60%) of ethyl 2-acetylamino-2-cyanopentanoate
  10. 10
    أخرىare obtained

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091203B2uspto-grants-2006_08