Acetic Acid → Ethyl 2,6-dicyano-3-methylhex-2-enoate

HRID 1248747ノート

反応式

HRID 1248747 の反応式
[C:1]([CH2:3][CH2:4][CH2:5][C:6]([CH3:8])=O)#[N:2].[C:9]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])#[N:10].C(O)(=O)C.C([O-])(=O)C.[NH4+]>C1(C)C=CC=CC=1>[CH2:15]([O:14][C:12](=[O:13])[C:11]([C:9]#[N:10])=[C:6]([CH3:8])[CH2:5][CH2:4][CH2:3][C:1]#[N:2])[CH3:16]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 7764Ethyl cyanoacetateHCID 82611Hexanenitrile, 5-oxo-HCID 517165Ammonium Acetate

生成物 1

HCID 54500111Ethyl 2,6-dicyano-3-methylhex-2-enoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of methyl 3-cyanopropyl ketone (55.5 g, 0.5 mole), ethyl cyanoacetate (56.5 g, 0.5 mole), acetic acid (6.0 g, 0.1 mole), ammonium acetate (3.85 g, 0.05 mole) and toluene (50 ml) was refluxed while azeotropically removing the water of reaction formed. After 10 hours the solution was vacuum distilled and a fraction (b.p. 145° C.-153° C., 0.5 torr) was collected. Total yield was 77.0 g or 74.7 percent. Analysis by infrared spectroscopy confirmed the product's identity as:

後処理

  1. temperaturewas refluxed
  2. customwhile azeotropically removing
  3. customthe water of reaction
  4. customformed
  5. distillationvacuum distilled
  6. customa fraction (b.p. 145° C.-153° C., 0.5 torr) was collected

出典と根拠

ORDレコード
ord-51ec1de1199247a28bbbdefc3a56315e
出典データセット
uspto-grants-1985_06
特許番号
US04525577

反応ノート

読み込み中…