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Dimethylformamide → 2,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)benzenamine

HRID 463452
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HRID 463452 반응식
CN(C)C=O.Cl.[NH2:7][C:8]1[C:13]([Cl:14])=[CH:12][C:11]([OH:15])=[C:10]([Cl:16])[CH:9]=1.[OH-].[K+].[F:19][C:20]([F:24])=[C:21]([F:23])[F:22]>O>[Cl:14][C:13]1[CH:12]=[C:11]([O:15][C:21]([F:23])([F:22])[CH:20]([F:24])[F:19])[C:10]([Cl:16])=[CH:9][C:8]=1[NH2:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8301TetrafluoroethyleneHCID 14797Potassium HydroxideHCID 135172884-Amino-2,5-dichlorophenol hydrochloride

생성물 1

HCID 135172892,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)benzenamine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
85 °C

실험 절차

A mixture of 100 ml dimethylformamide (DMF), 75 g (0.035 mole) 4-amino-2,5-dichlorophenol, hydrochloride, and 3.0 g (0.05 mole) KOH (pellets ground to powder) was placed in a 500 ml 3-necked round bottom flask fitted with a mechanical stirrer, thermometer and reflux condenser and was stirred for about 1 hour. It was then heated to 85° C. with stirring and 6.0 g (0.06 mole) of tetrafluoroethylene was bubbled in while heating at 85°-90° C. The addition took about 10 minutes. The reactor and contents were cooled in an ice water bath and 200 ml of water were added. The product was extracted with 200 ml methylene chloride and then again with 100 ml methylene chloride. The extracts were combined and the solvents removed by vacuum distillation. A residue (7 g) remained.

후처리

  1. customwas placed in a 500 ml 3-necked round bottom flask
  2. customfitted with a mechanical stirrer
  3. temperaturethermometer and reflux condenser
  4. stirringwith stirring
  5. temperaturewhile heating at 85°-90° C
  6. additionThe addition
  7. waittook about 10 minutes
  8. temperatureThe reactor and contents were cooled in an ice water bath
  9. extractionThe product was extracted with 200 ml methylene chloride
  10. customthe solvents removed by vacuum distillation

출처 및 근거

ORD 기록
ord-987540b5256b4e5b9ac74ffb1b84ae6a
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04518804

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