4-Aminophenol → 4-(2-Chloro-1,1-difluoroethoxy)benzeneamine

HRID 1655549

반응식

HRID 1655549 반응식
[CH:1]1[C:6]([NH2:7])=[CH:5][CH:4]=[C:3]([OH:8])[CH:2]=1.Cl[C:10]([F:14])([F:13])[CH2:11][Cl:12].C([O-])([O-])=O.[K+].[K+].C(#N)C>O>[Cl:12][CH2:11][C:10]([F:14])([F:13])[O:8][C:3]1[CH:4]=[CH:5][C:6]([NH2:7])=[CH:1][CH:2]=1

참가 물질

6

반응물 4

HCID 4034-AminophenolHCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 154421,2-Dichloro-1,1-difluoroethane

생성물 1

HCID 197927004-(2-Chloro-1,1-difluoroethoxy)benzeneamine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.5 g (22.9 mmol) of p-aminophenol, 3.09 g (22.9 mmol) of 1,2-dichloro-1,1-difluoroethane, 5.48 g (39.6 mmol) of K2CO3 and 40 ml of dry acetonitrile were stirred together at room temperature for 5 days. The mixture was poured into water and extracted two times into ether. The combined ether extracts were washed with water, dried over MgSO4 and filtered: HCl gas was bubbled into the ether solution causing the above-named aniline to precipitate as the hydrochloride salt, which was collected by filtration and recrystallized twice from CH3CN to give 0.9 g (16 percent of theoretical d 245°-250° C.) of a white solid.

후처리

  1. extractionextracted two times into ether
  2. washThe combined ether extracts were washed with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customHCl gas was bubbled into the ether solution
  6. customto precipitate as the hydrochloride salt, which
  7. filtrationwas collected by filtration
  8. customrecrystallized twice from CH3CN
  9. customto give 0.9 g (16 percent of theoretical d 245°-250° C.) of a white solid

출처 및 근거

ORD 기록
ord-c511a8c8feb8478d9e51ff3b4f62f5c5
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250690

연결된 노트

불러오는 중…