Реакция #41196

Уравнение реакции

cyclobutanone

hydrazinecarboxylic acid tert-butyl ester

→

N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester

Выход 81.2%

Растворители

hexane

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураto reflux for 2 hours
3. 3
   ТемператураAfter cooling down
4. 4
   Другоеa precipitate formed
5. 5
   Фильтрацияthe solid was filtered under vacuum
6. 6
   workup.ADDITIONIsopropanol (10 mL) and hexane (100 mL) were added to the solid
7. 7
   Другоеthe mixture was put on the rotary evaporator under vacuum until a slurry
8. 8
   ФильтрацияAfter filtration
9. 9
   Промывкаthe solid was washed with hexane twice
10. 10
    Другоеdried in vacuo

Методика

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.

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