Sodium Hydroxide → alpha-(3,4-Dichlorophenyl)-alpha-(2,6-dichloro-4-nitrophenyl)acetonitrile

HRID 321983ノート

反応式

HRID 321983 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[Cl:11])[CH2:5][C:6]#[N:7].Br[C:13]1[C:18]([Cl:19])=[CH:17][C:16]([N+:20]([O-:22])=[O:21])=[CH:15][C:14]=1[Cl:23].[OH-].[Na+]>CS(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]([C:13]2[C:14]([Cl:23])=[CH:15][C:16]([N+:20]([O-:22])=[O:21])=[CH:17][C:18]=2[Cl:19])[C:6]#[N:7])[CH:8]=[CH:9][C:10]=1[Cl:11]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 76690(3,4-Dichlorophenyl)acetonitrileHCID 99933122-Bromo-1,3-dichloro-5-nitrobenzene

生成物 1

HCID 22008581alpha-(3,4-Dichlorophenyl)-alpha-(2,6-dichloro-4-nitrophenyl)acetonitrile収率 67%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

To 150 ml of 20% hydrous DMSO were added 6.15 g of 3,4-dichlorobenzyl cyanide, 8.13 g of 4-bromo-3,5-dichloronitrobenzene and 1.50 g of sodium hydroxide. The reaction was allowed to proceed for one hour at temperatures ranging from 60 to 70° C. After completion of the reaction, DMSO was removed, and the residue was dissolved in 50 ml of toluene. The solution was washed with water, dried and concentrated. To the concentrate was added ethyl alcohol to cause crystallization to afford the titled compound in a yield of 67%, m.p.171-172° C.

後処理

  1. customranging from 60 to 70° C
  2. customwas removed
  3. dissolutionthe residue was dissolved in 50 ml of toluene
  4. washThe solution was washed with water
  5. customdried
  6. concentrationconcentrated
  7. additionTo the concentrate was added ethyl alcohol
  8. customcrystallization

出典と根拠

ORDレコード
ord-d5d57baf1dee47728c1cadcd99808389
出典データセット
uspto-grants-2001_04
特許番号
US06211178B1

反応ノート

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