반응 #41196

반응 방정식

cyclobutanone

hydrazinecarboxylic acid tert-butyl ester

→

N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester

수율 81.2%

용매

hexane

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to reflux for 2 hours
3. 3
   온도After cooling down
4. 4
   기타a precipitate formed
5. 5
   여과the solid was filtered under vacuum
6. 6
   workup.ADDITIONIsopropanol (10 mL) and hexane (100 mL) were added to the solid
7. 7
   기타the mixture was put on the rotary evaporator under vacuum until a slurry
8. 8
   여과After filtration
9. 9
   세척the solid was washed with hexane twice
10. 10
    기타dried in vacuo

실험 절차

The reaction mixture of cyclobutanone (15 g, 214 mmol) and hydrazinecarboxylic acid tert-butyl ester (28.3 g, 214 mmol) in hexane (225 mL) was heated to reflux for 2 hours. After cooling down, a precipitate formed and the solid was filtered under vacuum. Isopropanol (10 mL) and hexane (100 mL) were added to the solid and the mixture was put on the rotary evaporator under vacuum until a slurry was generated. After filtration, the solid was washed with hexane twice and dried in vacuo to afford N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester (32 g, 81%) as white solid which was used without further purification.

출처