2,3-Dichlorophenol → 4-Chloro-5-(2,3-dichlorophenoxy)-2-nitroaniline

HRID 1109742ノート

反応式

HRID 1109742 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].[Cl:10][C:11]1[C:17](Cl)=[CH:16][C:14]([NH2:15])=[C:13]([N+:19]([O-:21])=[O:20])[CH:12]=1.[OH-].[K+]>O>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][C:17]1[C:11]([Cl:10])=[CH:12][C:13]([N+:19]([O-:21])=[O:20])=[C:14]([CH:16]=1)[NH2:15]

参加物

5

反応物 3

HCID 113342,3-DichlorophenolHCID 14797Potassium HydroxideHCID 811494,5-Dichloro-2-nitroaniline

生成物 1

HCID 143492654-Chloro-5-(2,3-dichlorophenoxy)-2-nitroaniline

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of 171 g of 2,3-dichlorophenol and 186 g of 4,5-dichloro-2-nitroaniline is heated to 150° C. 101 g of a 50% potassium hydroxide solution are added dropwise to the dark-red liquid over a period of 1 hour. The water of reaction formed is distilled off with a small amount of phenol. The reaction mixture is stirred overnight at 150° C. and then, at that temperature, 450 ml of dimethylformamide are added. The solution is allowed to cool and is all poured onto a mixture of 3 1 of water and 150 ml of concentrated sodium hydroxide solution. The greenish suspension is stirred at room temperature for 1 hour, and the crystals that form are filtered off and washed neutral with water and then dried. The still moist yellowish crystals are used in crude form in the next reaction step.

後処理

  1. customformed
  2. distillationis distilled off with a small amount of phenol
  3. additionat that temperature, 450 ml of dimethylformamide are added
  4. temperatureto cool
  5. additionall poured onto a mixture of 3 1 of water and 150 ml of concentrated sodium hydroxide solution
  6. stirringThe greenish suspension is stirred at room temperature for 1 hour
  7. filtrationthe crystals that form are filtered off
  8. washwashed neutral with water
  9. customdried
  10. customin the next reaction step

出典と根拠

ORDレコード
ord-fa7aafb815df42a5a104f4b7f7a71197
出典データセット
uspto-grants-1994_06
特許番号
US05322853

反応ノート

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