HCID 13187346、化合物 → HCID 13187347、化合物

HRID 1379974ノート

反応式

HRID 1379974 の反応式
[CH3:1][O:2][Na].Cl[CH2:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[CH2:7]>CO>[CH3:1][O:2][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[CH2:7]

参加物

4

反応物 2

HCID 13187346HCID 13187346、化合物HCID 178418582HCID 178418582、化合物

生成物 1

HCID 13187347HCID 13187347、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a CH3ONa-solution from 6.9 g (0.3 gramatom) Na and 600 ml absolute CH3OH are added 59.3 g (0.3 Mol) 4(1-chloromethyl-ethenyl)-nitrobenzene, the reaction mixture heated under reflux for 2 hours and then evaporated to dryness. The residue is digested with diethylether, the ethereal solution filtered and the filtrate concentrated by evaporation. The residue is then chromatographed on silica gel (eluant n-hexane/diethylether 1:1) to give the title compound in analytically pure form (Rf=0.37 on silica gel with CHCl3).

後処理

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 2 hours
  3. customevaporated to dryness
  4. filtrationthe ethereal solution filtered
  5. concentrationthe filtrate concentrated by evaporation
  6. customThe residue is then chromatographed on silica gel (eluant n-hexane/diethylether 1:1)

出典と根拠

ORDレコード
ord-a78641322b10404080059f284fba1f38
出典データセット
uspto-grants-1986_04
特許番号
US04579585

反応ノート

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