Triethylamine → 1,3-Dimethyl-4,6-dioxo-2-thioxo-N-[4-(4-trifluoromethylphenoxy)phenyl]perhydropyrimidine-5-carboxamide

HRID 1194657노트

반응식

HRID 1194657 반응식
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:18]=[CH:17][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[O:16])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.[CH3:21][N:22]1[C:29](=[O:30])[CH2:28][C:26](=[O:27])[N:25]([CH3:31])[C:23]1=[S:24].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:31][N:25]1[C:26](=[O:27])[CH:28]([C:15]([NH:14][C:11]2[CH:12]=[CH:13][C:8]([O:7][C:6]3[CH:17]=[CH:18][C:3]([C:2]([F:19])([F:20])[F:1])=[CH:4][CH:5]=3)=[CH:9][CH:10]=2)=[O:16])[C:29](=[O:30])[N:22]([CH3:21])[C:23]1=[S:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5989481,3-Dimethyl-2-sulfanylidene-1,3-diazinane-4,6-dioneHCID 131894424-(4'-Trifluoromethylphenoxy)phenyl isocyanate

생성물 1

HCID 140533731,3-Dimethyl-4,6-dioxo-2-thioxo-N-[4-(4-trifluoromethylphenoxy)phenyl]perhydropyrimidine-5-carboxamide

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

4-(4'-Trifluoromethylphenoxy)phenyl isocyanate (3.7 g.) was added to a stirred mixture of 1,3-dimethyl-2-thiobarbituric acid (2.3 g.) and triethylamine (1.7 ml.) in dry benzene (30 ml.). The mixture was refluxed for 12 hours. The mixture was evaporated in vacuo. Diethyl ether (10 ml.) was added to the gummy residue and the mixture was acidified with 1N hydrochloric acid. The mixture was filtered and the solid was washed with water and then ethanol.

후처리

  1. temperatureThe mixture was refluxed for 12 hours
  2. customThe mixture was evaporated in vacuo
  3. additionDiethyl ether (10 ml.) was added to the gummy residue
  4. filtrationThe mixture was filtered
  5. washthe solid was washed with water

출처 및 근거

ORD 기록
ord-1fc0aa96892f4da8a81efcacb95ef557
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816460

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