1-Methylthio-1-methylamino-2-nitroethylene → 1-[3-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethylene

HRID 34781

반응식

HRID 34781 반응식
[F:1][C:2]([F:20])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][CH2:16][NH2:17])[N:8]=1.[CH3:21][NH:22][C:23](SC)=[CH:24][N+:25]([O-:27])=[O:26]>C(#N)C>[F:20][C:2]([F:1])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][CH2:16][NH:17][C:23]([NH:22][CH3:21])=[CH:24][N+:25]([O-:27])=[O:26])[N:8]=1

참가 물질

4

반응물 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 212987114-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(3-aminopropylthio)pyrimidine

생성물 1

HCID 704179461-[3-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethylene수율 26.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(3-aminopropylthio)pyrimidine (0.31 g.) in acetonitrile (5 ml.) was treated with 1-methylamino-1-methylthio-2-nitroethylene (0.15 g.) and the mixture heated under reflux for 18 hours. The hot solution was filtered and cooled and the solid which crystallised was collected and recrystallised from ethanol to give 1-[3-(4-[2-(2,2,2-trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethylene (0.11 g.), m.p. 189°-191°.

후처리

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 18 hours
  3. filtrationThe hot solution was filtered
  4. temperaturecooled
  5. customthe solid which crystallised
  6. customwas collected
  7. customrecrystallised from ethanol

출처 및 근거

ORD 기록
ord-55894688c5ab4642bc637db5c9cec5c3
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762932

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