Ethanol → 1-Propene-1,1,3-tricarbonitrile, 2-phenyl-

HRID 893566ノート

反応式

HRID 893566 の反応式
[C:1]([CH2:9][C:10]#[N:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12](#[N:16])[CH2:13][C:14]#[N:15].C([O-])(=O)C.[NH4+].C(O)C>O.Cl>[C:2]1([C:1]([CH2:9][C:10]#[N:11])=[C:13]([C:12]#[N:16])[C:14]#[N:15])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 702EthanolHCID 8010MalononitrileHCID 64799BenzoylacetonitrileHCID 517165Ammonium Acetate

生成物 1

HCID 46214401-Propene-1,1,3-tricarbonitrile, 2-phenyl-

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

A mixture of benzoylacetonitrile (9.94 g, 0.0685 mole), malononitrile (11.3 g, 0.17 mole), ammonium acetate (5.4 g, 0.07 mole) and ethanol (100 mL) was heated at reflux for 1.5 hours. After cooling to room temperature, the reaction mixture was diluted with water (50 mL) and concentrated hydrochloric acid (7.5 mL) was added dropwise over 5 minutes. The resulting precipitate was collected by filtration and washed with water and ligroin. The yield was 10.0 g (76%), m.p. 92°-98° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 1.5 hours
  3. additionwas added dropwise over 5 minutes
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water and ligroin

出典と根拠

ORDレコード
ord-a6611c7252424958ad7f34ace9da2493
出典データセット
uspto-grants-1992_06
特許番号
US05126312

反応ノート

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