2-Propenenitrile, 3-hydroxy- → 3-(2,3-Dichlorophenacylamino)acrylonitrile

HRID 703266

反応式

HRID 703266 の反応式
Cl.[Cl:2][C:3]1[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5](=[O:8])[CH2:6][NH2:7].O[CH:15]=[CH:16][C:17]#[N:18].[Na]>C(O)C>[Cl:2][C:3]1[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5](=[O:8])[CH2:6][NH:7][CH:15]=[CH:16][C:17]#[N:18]

参加物

5

反応物 3

HCID 30540732-Propenenitrile, 3-hydroxy-HCID 5360545SodiumHCID 22151845Ethanone, 2-amino-1-(2,3-dichlorophenyl)-, hydrochloride

生成物 1

HCID 679440943-(2,3-Dichlorophenacylamino)acrylonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2 g of 2,3-dichlorophenacylamine hydrochloride, 1 g of 3-hydroxyacrylonitrile, sodium salt, and 20 ml of ethanol are heated for 2 hours under reflux. The reaction mixture is concentrated by evaporation and the oily residue is purified by column chromatography (silica gel; elution with a 4:1 mixture of toluene/ethyl acetate), affording 3-(2,3-dichlorophenacylamino)acrylonitrile in the cis/trans ratio of 5:1. Melting point: 122°-125° C.

後処理

  1. temperatureunder reflux
  2. concentrationThe reaction mixture is concentrated by evaporation
  3. customthe oily residue is purified by column chromatography (silica gel
  4. washelution
  5. additionwith a 4:1 mixture of toluene/ethyl acetate),

出典と根拠

ORDレコード
ord-296fccb88ba5466da8ea50a16aeef931
出典データセット
uspto-grants-1991_01
特許番号
US04981990

関連ノート

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