반응 #2066029

반응 방정식

methyl cyanoacetate

methyl cyanoacetate

piperidine

3-(4-chloro-3-formylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

diisopropyl ether

→

3-[4-Chloro-3-(2-cyano-2-methoxycarbonylethenyl)-phenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도refluxing
2. 2
   workup.WAITwas continued for a further 5 hours
3. 3
   기타The reaction mixture was evaporated down
4. 4
   기타the oil obtained
5. 5
   기타was chromatographed (dichloromethane)
6. 6
   기타The solid obtained
7. 7
   기타isolated
8. 8
   세척washed with petroleum ether
9. 9
   기타dried

실험 절차

0.97 ml of methyl cyanoacetate and 0.3 ml of piperidine were added to a solution of 3.3 g of 3-(4-chloro-3-formylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine in 100 ml of tetrahydrofuran. After the mixture had been stirred for 5 hours at the reflux temperature, a further 0.97 ml of methyl cyanoacetate was added and refluxing was continued for a further 5 hours. The reaction mixture was evaporated down and the oil obtained was chromatographed (dichloromethane). The solid obtained was stirred with diisopropyl ether, isolated, washed with petroleum ether and dried.

출처