Aluminum(III) Chloride → 3-(2,4-Dichlorophenoxy)phenol

HRID 1759216ノート

反応式

HRID 1759216 の反応式
[Cl:1][C:2]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([O:11]C)[CH:8]=[CH:9][CH:10]=1.[Cl-].[Al+3].[Cl-].[Cl-]>ClC1C=CC=CC=1>[Cl:1][C:2]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 205325313-(2,4-Dichlorophenoxy)-anisole

生成物 1

HCID 127961723-(2,4-Dichlorophenoxy)phenol収率 89.8%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
60 °C

実験手順

18.8 g of 3-(2,4-dichlorophenoxy)-anisole are added to a suspension of 37 g of anhydrous aluminium chloride in 80 ml of chlorobenzene and the mixture is stirred for 1 day at 60° C. The still hot solution is poured onto ice. The resulting mixture is extracted with toluene and the toluene solution is extracted with 2 N sodium hydroxide solution. The product is precipitated by acidifying the sodium hydroxide solution with dilute hydrochloric acid and extracted with toluene. The toluene solution is concentrated and the residue distilled in vacuo, affording 16 g of 3-(2,4-dichlorophenoxy)-phenol in the form of a colourless oil with a boiling point of 140°-145° C./0.05 torr. Using the corresponding chlorophenols as starting materials, it is possible to obtain the starting materials required for the production of the compounds of the formulae (302) to (304):

後処理

  1. additionThe still hot solution is poured onto ice
  2. extractionThe resulting mixture is extracted with toluene
  3. extractionthe toluene solution is extracted with 2 N sodium hydroxide solution
  4. customThe product is precipitated
  5. extractionextracted with toluene
  6. concentrationThe toluene solution is concentrated
  7. distillationthe residue distilled in vacuo

出典と根拠

ORDレコード
ord-74dfde391d114546b02914769899f6dd
出典データセット
uspto-grants-1982_07
特許番号
US04339462

反応ノート

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