反応 #4424

反応方程式

2-chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

piperazine

→

3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-2-(1-piperazinyl)-4-(2,4,6-trimethylphenylimino)pyrimidine

収率 57.3%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The mixture was refluxed for 3 hours
2. 2
   その他The mixture was evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in chloroform
4. 4
   洗浄washed with aqueous sodium bicarbonate solution
5. 5
   乾燥The organic layer was dried over magnesium sulfate
6. 6
   その他evaporated
7. 7
   その他The residue was chromatographed on silica gel using
8. 8
   workup.ADDITIONa mixture of chloroform and methanol (95:5)

実験手順

To a suspension of 2-chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (1.07 g) in ethanol (10 ml) was added piperazine (0.70 g). The mixture was refluxed for 3 hours, cooled to ambient temperature. The mixture was evaporated, and the residue was dissolved in chloroform and washed with aqueous sodium bicarbonate solution. The organic layer was dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel using a mixture of chloroform and methanol (95:5) to give 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-2-(1-piperazinyl)-4-(2,4,6-trimethylphenylimino)pyrimidine (0.69 g).

出典