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

HRID 728988
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HRID 728988 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, theethanol 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, theethanol 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-82b03bc4d3b149869312c559bdf2b66a
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05051434

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