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1,1-Bis(methylthio)-2-nitroethylene → 1-{1-(2-Chloro-5-pyridyl)ethylamino}-1-methylthio-2-nitroethylene

HRID 1091072
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HRID 1091072 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([NH2:10])[CH3:9])=[CH:4][N:3]=1.[CH3:11][S:12][C:13](SC)=[CH:14][N+:15]([O-:17])=[O:16]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([NH:10][C:13]([S:12][CH3:11])=[CH:14][N+:15]([O-:17])=[O:16])[CH3:9])=[CH:4][N:3]=1
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참가 물질

4

반응물 2

HCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 157456051-(6-Chloropyridin-3-yl)ethan-1-amine

생성물 1

HCID 727435041-{1-(2-Chloro-5-pyridyl)ethylamino}-1-methylthio-2-nitroethylene수율 40.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1-(2-chloro-5-pyridyl)ethylamine (4.7 g), 1,1-bis-methylthio-2-nitroethylene (5.0 g) and ethanol (50 ml) was refluxed under heating until the generation of mercaptan ceased. Then, the ethanol was distilled off from the mixture under reduced pressure and the resulting residue was purified on a chromatographic column (the eluent mixture=ethanol+chloroform) to obtain the desired 1-{1-(2-chloro-5-pyridyl)ethylamino}-1-methylthio-2-nitroethylene (3.3 g) having a melting point in the range of from 136° to 140° C.

후처리

  1. temperaturewas refluxed
  2. distillationThen, the ethanol was distilled off from the mixture under reduced pressure
  3. customthe resulting residue was purified on a chromatographic column (the eluent mixture=ethanol+chloroform)

출처 및 근거

ORD 기록
ord-2fb33fef6e5040c7ab9e9f3bbed36727
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05084467

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