반응 #93427

반응 방정식

water

n-propyl iodide

6-(3,4-dimethoxyphenyl)-3-methyl-2,4(1H,3H)-pyrimidinedione

sodium hydride

→

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

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도cooled to 0° C
2. 2
   workup.STIRRINGwith stirring
3. 3
   workup.WAITwhich was continued at 0° C. for 2 hours and at ambient temperature for 3 hours
4. 4
   추출the reaction mixture was extracted with ethyl acetate
5. 5
   추출The organic extract
6. 6
   세척was washed with water
7. 7
   건조dried over magnesium sulfate
8. 8
   기타evaporated under reduced pressure
9. 9
   기타The residue was triturated with diisopropyl ether
10. 10
    기타the resulting precipitates
11. 11
    여과were collected by filtration

실험 절차

To a solution of 6-(3,4-dimethoxyphenyl)-3-methyl-2,4(1H,3H)-pyrimidinedione (3.0 g) in N,N-dimethylformamide (30 ml) was added sodium hydride (60% in oil, 0.5 g). The mixture was heated at 60° C. with stirring for 20 minutes and cooled to 0° C. To the mixture was added n-propyl iodide (15 ml) with stirring, which was continued at 0° C. for 2 hours and at ambient temperature for 3 hours. After addition of water, the reaction mixture was extracted with ethyl acetate. The organic extract was washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether and the resulting precipitates were collected by filtration to give 6-(3,4-dimethoxyphenyl)-3-methyl-2-propoxy-4(3H)-pyrimidinone (1.15 g) as by-product.

출처