Cyclopropylamine → N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine

HRID 1200247노트

반응식

HRID 1200247 반응식
[CH3:1][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15](SC)=[CH:16][N+:17]([O-:19])=[O:18])[N:9]=1)[CH3:3].[CH:22]1([NH2:25])[CH2:24][CH2:23]1>C(O)C>[CH3:3][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]([NH:25][CH:22]2[CH2:24][CH2:23]2)=[CH:16][N+:17]([O-:19])=[O:18])[N:9]=1)[CH3:1]

참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 678972721-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene

생성물 1

HCID 70363512N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A reaction mixture, prepared from 1-[2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene, cyclopropylamine and ethanol, was heated to refluxing temperature for about three hours. The solvent was then removed by evaporation and the resulting residue was chromatographed over silica using a gradient elution technique. The desired compound was eluted with a 5:95 methanol:ethyl acetate solvent mixture. Removal of the solvent yielded N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine which melted at 128.5°-131.5° C. after recrystallization from a methanol/ethyl acetate solvent mixture.

후처리

  1. temperaturewas heated
  2. temperatureto refluxing temperature for about three hours
  3. customThe solvent was then removed by evaporation
  4. customthe resulting residue was chromatographed over silica using
  5. washa gradient elution technique
  6. washThe desired compound was eluted with a 5:95 methanol
  7. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-2cca6b5a100f4a8892a8feaed54955d1
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904792

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