Benzaldehyde → HCID 20296018、化合物

HRID 1389930

反応式

HRID 1389930 の反応式
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([Cl:17])=[CH:12][C:11]=1[NH2:18].[C-:19]#[N:20].[K+]>[Cl-].[Zn+2].[Cl-].O>[Cl:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([Cl:17])=[CH:12][C:11]=1[NH:18][CH:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:19]#[N:20]

参加物

6

反応物 3

HCID 240BenzaldehydeHCID 9032Potassium CyanideHCID 124872,4,5-Trichloroaniline

生成物 1

HCID 20296018HCID 20296018、化合物

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a stirred mixture of 53 parts of benzaldehyde in 820 parts of water are added successively 78.6 parts of 2,4,5-trichlorobenzenamine, 81.8 parts of zinc chloride and 32.6 parts of potassium cyanide and the whole is stirred for 18 hours at 50° C. The reaction mixture is cooled to room temperature. The precipitated product is filtered off, triturated in 1000 parts of water, filtered off again and dissolved in 750 parts of trichloromethane. The solution is washed twice with water, dried, filtered and evaporated. The solid residue is triturated in petroleum ether, filtered off again and dried, yielding 83.1 parts of α-[(2,4,5-trichlorophenyl)amino]benzeneacetonitrile; mp. 123.7° C.

後処理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. filtrationThe precipitated product is filtered off
  3. customtriturated in 1000 parts of water
  4. filtrationfiltered off again
  5. dissolutiondissolved in 750 parts of trichloromethane
  6. washThe solution is washed twice with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe solid residue is triturated in petroleum ether
  11. filtrationfiltered off again
  12. customdried

出典と根拠

ORDレコード
ord-d1698bafec5a4e2fb43185c9e8bd4d09
出典データセット
uspto-grants-1981_01
特許番号
US04246429

関連ノート

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