반응 #93436

반응 방정식

6-(3,4-dimethoxyphenyl)-2-isopropoxy-3-methyl-4(3H)-pyrimidinone

phosphorus pentasulfide

→

3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-thioxo-2(1H)-pyrimidinone

수율 12.3%

용매

pyridine

반응 조건

후처리

1. 1
   온도was refluxed for 13 hours
2. 2
   기타The reaction mixture was evaporated under reduced pressure
3. 3
   세척The residue was washed with 1N-hydrochloric acid
4. 4
   추출extracted with chloroform
5. 5
   세척The extract was washed with water
6. 6
   건조dried over magnesium sulfate
7. 7
   기타evaporated under reduced pressure
8. 8
   기타The residue was triturated in ethanol
9. 9
   기타the resulting precipitate was triturated again in chloroform
10. 10
    여과collected by filtration

실험 절차

A mixture of 6-(3,4-dimethoxyphenyl)-2-isopropoxy-3-methyl-4(3H)-pyrimidinone (2.5 g) and phosphorus pentasulfide (3.5 g) in pyridine (50 ml) was refluxed for 13 hours with stirring. The reaction mixture was evaporated under reduced pressure. The residue was washed with 1N-hydrochloric acid and extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated in ethanol and the resulting precipitate was triturated again in chloroform and collected by filtration to give 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-thioxo-2(1H)-pyrimidinone (0.27 g).

출처