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2,6-Dimethylaniline → (2,6-Dimethylanilino)acetonitrile

HRID 2285942
ノート
印刷プレビュー

反応式

HRID 2285942 の反応式
C1(S([O-])(=O)=O)C=CC=CC=1.[C:11](#[N:13])[CH3:12].[CH3:14][C:15]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:16]=1[NH2:17]>C(OCC)(=O)C>[CH3:14][C:15]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:16]=1[NH:17][CH2:12][C:11]#[N:13]
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 68962,6-DimethylanilineHCID 86738343HCID 86738343、化合物

生成物 1

HCID 20478053(2,6-Dimethylanilino)acetonitrile

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A solution of 158.5 g (0.804 mol) of benzenesulphonate-acetonitrile in 200 ml of ethyl acetate is run dropwise into a solution of 193.6 g (1.608 mols) of 2,6-dimethyl-aniline in 400 ml of ethyl acetate. The mixture is heated under reflux for 3 hours, cooled and the excess aniline benzenesulphonate is filtered off. The filtrate is evaporated to dryness. The residue is taken up in ether. Insoluble material is again filtered off and discarded. The ether is evaporated to dryness. The residue is taken up in a mixture of petroleum ether/benzene (3:4 v/v). The crystals which form are filtered off.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. temperaturecooled
  4. filtrationthe excess aniline benzenesulphonate is filtered off
  5. customThe filtrate is evaporated to dryness
  6. filtrationInsoluble material is again filtered off
  7. customThe ether is evaporated to dryness
  8. additionThe residue is taken up in a mixture of petroleum ether/benzene (3:4 v/v)
  9. filtrationThe crystals which form are filtered off

出典と根拠

ORDレコード
ord-80aecad225ff4701acbe0d42ff2af916
出典データセット
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04325964

反応ノート

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