반응 #2066035

ord-7115392c8f4f4abea9e8aa8819320a7d

반응 방정식

CCOC(=O)NN
ethyl hydrazinecarboxylate
Cn1c(C(F)(F)F)cc(=O)n(-c2ccc(Cl)c(C=O)c2)c1=O
3-[4-chloro-3-formylphenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine
Cc1ccc(S(=O)(=O)O)cc1
p-toluenesulfonic acid
CCOC(=O)NN=Cc1cc(-n2c(=O)cc(C(F)(F)F)n(C)c2=O)ccc1Cl
3-(4-Chloro-3-ethoxycarbonylhydrazonomethylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척the solution was washed once with water
  2. 2
    건조the organic phase was dried over sodium sulfate
  3. 3
    기타evaporated down
  4. 4
    기타The precipitate was isolated
  5. 5
    세척washed with petroleum ether
  6. 6
    기타dried

실험 절차

1.0 g of ethyl hydrazinecarboxylate was 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 and 0.1 g of p-toluenesulfonic acid in 150 ml of toluene. After 2 hours, the solution was washed once with water, the organic phase was dried over sodium sulfate and evaporated down and the residue was stirred with petroleum ether. The precipitate was isolated, washed with petroleum ether and dried.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06239074B1uspto-grants-2001_05