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

HRID 2287096노트

반응식

HRID 2287096 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 127961723-(2,4-Dichlorophenoxy)phenol수율 89.8%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

반응 조건

온도
60 °C

실험 절차

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):

후처리

  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

출처 및 근거

ORD 기록
ord-9d217ec678f042ebb11805fe775c64b5
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04268693

반응 노트

불러오는 중…