反応 #41196

反応方程式

cyclobutanone

hydrazinecarboxylic acid tert-butyl ester

→

N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester

収率 81.2%

溶媒

hexane

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度to reflux for 2 hours
3. 3
   温度After cooling down
4. 4
   その他a precipitate formed
5. 5
   ろ過the solid was filtered under vacuum
6. 6
   workup.ADDITIONIsopropanol (10 mL) and hexane (100 mL) were added to the solid
7. 7
   その他the mixture was put on the rotary evaporator under vacuum until a slurry
8. 8
   ろ過After filtration
9. 9
   洗浄the solid was washed with hexane twice
10. 10
    その他dried in vacuo

実験手順

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.

出典