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Malononitrile → 2-((3,4-Dimethoxyphenyl)methylene)propanedinitrile

HRID 1647711
ノート
印刷プレビュー

反応式

HRID 1647711 の反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[CH3:6][O:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[O:16][CH3:17])[CH:11]=O>C(O)C>[CH3:6][O:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[O:16][CH3:17])[CH:11]=[C:2]([C:1]#[N:5])[C:3]#[N:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8010MalononitrileHCID 8419Veratraldehyde

生成物 1

HCID 2196912-((3,4-Dimethoxyphenyl)methylene)propanedinitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of malononitrile (7.52 g) and 3,4-dimethoxybenzaldehyde (18.95 g) in ethanol (100 ml) was warmed to reflux temperature with stirring. The orange solution was removed from the heat and piperidine (0.5 ml) added down the condenser. Once the vigorous reaction had subsided, the reaction mixture was reheated to reflux temperature and this maintained for 35 minutes. Copious quantities of a bright yellow solid had appeared by this time. The mixture was cooled in an ice bath for 10 minutes and the yellow solid filtered off, washed with ethanol and ether and dried in vacuo at 70° C. yielding 3,4-dimethoxy benzylidenemalononitrile, m.p.137° C.

後処理

  1. temperaturewas warmed
  2. temperatureto reflux temperature
  3. customThe orange solution was removed from the
  4. temperatureheat
  5. additionpiperidine (0.5 ml) added down the condenser
  6. customOnce the vigorous reaction
  7. temperatureto reflux temperature
  8. temperaturethis maintained for 35 minutes
  9. temperatureThe mixture was cooled in an ice bath for 10 minutes
  10. filtrationthe yellow solid filtered off
  11. washwashed with ethanol and ether
  12. customdried in vacuo at 70° C.

出典と根拠

ORDレコード
ord-4cc6771484df47dc80093b8380cc0ce4
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05434160

反応ノート

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