반응 #4424

반응 방정식

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

수율 57.3%

용매

ethanol

반응 조건

후처리

1. 1
   온도The mixture was refluxed for 3 hours
2. 2
   기타The mixture was evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in chloroform
4. 4
   세척washed with aqueous sodium bicarbonate solution
5. 5
   건조The organic layer was dried over magnesium sulfate
6. 6
   기타evaporated
7. 7
   기타The residue was chromatographed on silica gel using
8. 8
   workup.ADDITIONa mixture of chloroform and methanol (95:5)

실험 절차

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).

출처