반응 #1665

반응 방정식

4-benzoylbutyric acid

hydrazine

water

→

desired product

수율 39.0%

7-phenyl-1,2-diazapin-3-one

수율 39.0%

용매

toluene

toluene

Et2O

반응 조건

후처리

1. 1
   workup.ADDITIONwas added in one portion
2. 2
   온도the reaction was heated
3. 3
   온도The reaction mixture was cooled
4. 4
   세척washed with H2O (100 ml) and brine (100 ml)
5. 5
   추출The ether extract
6. 6
   건조was dried over anhydrous MgSO4
7. 7
   여과filtered
8. 8
   기타to yield an orange semisolid which
9. 9
   기타was triturated with ether

실험 절차

To a mixture of 10 g (0.052 mole) of 4-benzoylbutyric acid in 300 ml of toluene, hydrazine was added in one portion and the reaction was heated to reflux until all water had ceased to azeotrope. The reaction mixture was cooled and the toluene was stripped off in vacuo. The residue was dissolved in 200 ml Et2O and washed with H2O (100 ml) and brine (100 ml). The ether extract was dried over anhydrous MgSO4, filtered and stripped to yield an orange semisolid which was triturated with ether to yield 3.8 g (39%) of the desired product as a yellow solid.

출처