反応 #302874

反応方程式

2-phenyl acrylic acid methyl ester

3-amino-1,2,4-triazole

→

6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on

収率 19.0%

溶媒

n-butanol

反応条件

後処理

1. 1
   その他The solvent was removed under reduced pressure
2. 2
   workup.ADDITIONThe residue was treated with a small amount of ethanol and diethyl ether and cyclohexane
3. 3
   workup.ADDITIONwere added
4. 4
   その他The diethyl ether is slowly removed under reduced pressure
5. 5
   その他The crude 6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on precipitated during evaporation
6. 6
   その他was isolated by filtration
7. 7
   洗浄washed with diethyl ether
8. 8
   その他6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on was recrystallized from a small amount of ethanol

実験手順

A solution of 9.01 g (55.6 mmol) 2-phenyl acrylic acid methyl ester and 4.24 g (50.4 mmol) 3-amino-1,2,4-triazole in 41 ml n-butanol was refluxed for 24 hours. The solvent was removed under reduced pressure. The residue was treated with a small amount of ethanol and diethyl ether and cyclohexane were added. The diethyl ether is slowly removed under reduced pressure. The crude 6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on precipitated during evaporation, was isolated by filtration and washed with diethyl ether. 6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on was recrystallized from a small amount of ethanol. 2.04 g (19%) 6-phenyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrimidin-7-on was isolated (m.p. 184-186° C.).

出典