4-Aminophenol → 4-(1,1-Difluoro-2,2,2-trichloroethoxy)aniline

HRID 1655548

반응식

HRID 1655548 반응식
[CH:1]1[C:6]([NH2:7])=[CH:5][CH:4]=[C:3]([OH:8])[CH:2]=1.[H-].[Na+].[F:11][C:12](Cl)([F:17])[C:13]([Cl:16])([Cl:15])[Cl:14]>CS(C)=O>[F:11][C:12]([F:17])([O:8][C:3]1[CH:4]=[CH:5][C:6]([NH2:7])=[CH:1][CH:2]=1)[C:13]([Cl:16])([Cl:15])[Cl:14]

참가 물질

5

반응물 3

HCID 4034-AminophenolHCID 64261,1,1,2-Tetrachloro-2,2-difluoroethaneHCID 24758Sodium hydride

생성물 1

HCID 135292554-(1,1-Difluoro-2,2,2-trichloroethoxy)aniline

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

2.0 g (18.3 mmol) of p-aminophenol was added over a period of 10 minutes to a mixture of 0.48 g (20.1 mmol) of sodium hydride in 20 ml of dry DMSO. The mixture was stirred for 20 minutes. 3.73 g (18.3 mmol) of 1,1-difluoro-tetrachloroethane was added causing an exotherm to 47° C. The mixture was stirred at 60° C. for 2 hours, then poured into ice water. The brown solid was collected by filtration, dried, dissolved in ether and then HCl gas was bubbled into the solution causing the above-named aniline to precipitate as the hydrochloride salt. The white solid (4.4 g, 87 percent of theoretical d 250° C.) was collected by filtration.

후처리

  1. customto 47° C
  2. stirringThe mixture was stirred at 60° C. for 2 hours
  3. filtrationThe brown solid was collected by filtration
  4. customdried
  5. dissolutiondissolved in ether
  6. customHCl gas was bubbled into the solution
  7. customto precipitate as the hydrochloride salt
  8. filtrationThe white solid (4.4 g, 87 percent of theoretical d 250° C.) was collected by filtration

출처 및 근거

ORD 기록
ord-ce4291de36e44412b9bd74ae5712ae97
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250690

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