1,1-Bis(methylthio)-2-nitroethylene → HCID 54422628、化合物

HRID 1043518

反応式

HRID 1043518 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 54422628HCID 54422628、化合物収率 20.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9199bef9f13a44e7aa1e2e26d175dd72
出典データセット
uspto-grants-2013_10
特許番号
US08563546B2

関連ノート

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