1,1-Bis(methylthio)-2-nitroethylene → HCID 54422628, 화합물

HRID 1043518

반응식

HRID 1043518 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH3:11])=[CH:4][CH:3]=1.[N+:12]([CH:15]=[C:16](SC)[S:17][CH3:18])([O-:14])=[O:13]>C(O)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:10][CH3:11])[C:16]([S:17][CH3:18])=[CH:15][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 11137568N-((6-Chloropyridin-3-yl)methyl)ethanamine

생성물 1

HCID 54422628HCID 54422628, 화합물수율 20.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a 100 ml three necked round bottom flask was added N-((6-chloropyridin-3-yl)methyl)ethanamine (17.0 g, 0.1 mol), (2-nitroethene-1,1-diyl)bis(methylsulfane) (15.0 g, 0.09 mol), dry ethanol (50 mL). The mixture was refluxed. After completion, the reaction mixture was cooled to r.t. and concentrated under reduced pressure to obtain crude product as oil, which was purified by column chromatography to afford 5.3 g N-((6-chloropyridin-3-yl)methyl)-N-ethyl-1-(methylthio)-2-nitroethenamine in 18.5% yield.

후처리

  1. temperatureThe mixture was refluxed
  2. concentrationconcentrated under reduced pressure
  3. customto obtain crude product as oil, which
  4. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-9199bef9f13a44e7aa1e2e26d175dd72
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563546B2

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