4-Aminophenol → HCID 19792673, 화합물

HRID 1655550

반응식

HRID 1655550 반응식
[F:1][CH:2]=[C:3]([F:5])[F:4].[CH:6]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:8]([OH:13])[CH:7]=1.[OH-].[K+]>CN(C=O)C>[F:4][C:3]([F:5])([O:13][C:8]1[CH:9]=[CH:10][C:11]([NH2:12])=[CH:6][CH:7]=1)[CH2:2][F:1]

참가 물질

5

반응물 3

HCID 4034-AminophenolHCID 9665TrifluoroethyleneHCID 14797Potassium Hydroxide

생성물 1

HCID 19792673HCID 19792673, 화합물수율 25%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Gaseous trifluoroethylene was bubbled into a mixture of 7.0 g (64.1 mmol) of p-aminophenol, 0.7 g (12.8 mmol) of powdered KOH, and 70 ml dry DMF at 90° C. for 11/4 hours. The mixture was poured into ice water and extracted 2 times with ether. The combined ether layers were washed with diluted aqueous NaOH, washed with water, dried over MgSO4 and filtered. HCl was bubbled into the ether solution. The resulting gray solid was collected by filtration to give 3.6 g (25 percent of theoretical) of the above-named aniline as the HCl salt along with a 20 percent impurity of 4-(1,2-difluoroethenyloxy)benzene-amine.

후처리

  1. extractionextracted 2 times with ether
  2. washThe combined ether layers were washed with diluted aqueous NaOH
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customHCl was bubbled into the ether solution
  7. filtrationThe resulting gray solid was collected by filtration

출처 및 근거

ORD 기록
ord-b6d402b15d8b4fe29491860fc02ae96b
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250690

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