反応 #4771

反応方程式

ethyl acetate

1-acetyl-1-(3-nitrobenzyliden)acetone

benzamidine hydrochloride

triethylamine

→

5-acetyl-4-methyl-6-(3-nitrophenyl)-2-phenyl-1,6-dihydropyrimidine

収率 31.0%

溶媒

n-butanol

反応条件

後処理

1. 1
   温度was refluxed for 2 hours
2. 2
   洗浄washed with water (100 ml) and 5% hydrochloric acid (100 ml) successively
3. 3
   その他The solvent was evaporated
4. 4
   ろ過The crystals were collected by filtration
5. 5
   workup.ADDITIONadded
6. 6
   workup.ADDITIONa mixture of chloroform (100 ml) and water (100 ml)
7. 7
   その他The organic layer was evaporated in vacuo

実験手順

A mixture of 1-acetyl-1-(3-nitrobenzyliden)acetone (10 g), benzamidine hydrochloride (8.06 g) and triethylamine (8.4 ml) in n-butanol (100 ml) was refluxed for 2 hours. The reaction mixture was added ethyl acetate (100 ml), washed with water (100 ml) and 5% hydrochloric acid (100 ml) successively. The solvent was evaporated and the residue was stirred with ethyl acetate (100 ml) for 1 hour. The crystals were collected by filtration, added a mixture of chloroform (100 ml) and water (100 ml) and adjusted to pH 8.5 by saturated potassium carbonate. The organic layer was evaporated in vacuo to give 5-acetyl-4-methyl-6-(3-nitrophenyl)-2-phenyl-1,6-dihydropyrimidine (4.46 g).

出典