반응 #518102

반응 방정식

Potassium carbonate

2,4-dinitrophenoxyamine

3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

→

desired product

수율 52.0%

1-Amino-3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

수율 52.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타formed
2. 2
   기타were separated off
3. 3
   세척washed
4. 4
   세척The combined filtrates were washed twice
5. 5
   건조dried over sodium sulfate
6. 6
   농축concentrated
7. 7
   기타After crystallization

실험 절차

Potassium carbonate (1.0 g) and 2,4-dinitrophenoxyamine (0.8 g) were added to a solution of 3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (1.1 g) in 15 ml of ethyl acetate. The mixture was subsequently stirred for 15 hours at 55-60° C., whereupon the solids formed were separated off and washed using in each case 30 ml of ethyl acetate and diisopropyl ether. The combined filtrates were washed twice using in each case 25 ml of water, dried over sodium sulfate and then concentrated. After crystallization using 10 ml of diisopropyl ether, 0.6 g of the desired product was obtained. M.p.: >230° C.

출처