反応 #1665

反応方程式

4-benzoylbutyric acid

hydrazine

water

→

desired product

収率 39.0%

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

収率 39.0%

溶媒

toluene

toluene

Et2O

反応条件

後処理

1. 1
   workup.ADDITIONwas added in one portion
2. 2
   温度the reaction was heated
3. 3
   温度The reaction mixture was cooled
4. 4
   洗浄washed with H2O (100 ml) and brine (100 ml)
5. 5
   抽出The ether extract
6. 6
   乾燥was dried over anhydrous MgSO4
7. 7
   ろ過filtered
8. 8
   その他to yield an orange semisolid which
9. 9
   その他was triturated with ether

実験手順

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.

出典