Tin tetrachloride → 4-(2,5-Dichlorophenoxy)-3-fluoroaniline

HRID 1993818

반응식

HRID 1993818 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-])=O)=[CH:7][C:6]=1[F:14].[Sn](Cl)(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[F:14]

참가 물질

5

반응물 3

HCID 24287Tin tetrachlorideHCID 516892Sodium BicarbonateHCID 597980461-(2,5-Dichloro-phenoxy)-2-fluoro-4-nitro-benzene

생성물 1

HCID 289727064-(2,5-Dichlorophenoxy)-3-fluoroaniline

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

A mixture of 1-(2,5-dichloro-phenoxy)-2-fluoro-4-nitro-benzene (0.5 g, 1.7 mmol) and tin chloride (1.57 g, 8.3 mmol) in 30 ml of anhydrous ethanol was heated to 70° C. under argon and stirred for 4 hours. The solution was allowed to cool and then poured into ice. The solution was made slightly basic (pH 7-8) by addition of saturated aqueous sodium bicarbonate solution, then extracted with ethyl acetate. The organic phase was thoroughly washed with brine and dried treated with anhydrous sodium sulfate. Evaporation of the solvent left a yellow oily product which was used for the next step without further purification.

후처리

  1. temperatureto cool
  2. additionpoured into ice
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was thoroughly washed with brine
  5. customdried
  6. additiontreated with anhydrous sodium sulfate
  7. customEvaporation of the solvent
  8. waitleft a yellow oily product which
  9. customwas used for the next step without further purification

출처 및 근거

ORD 기록
ord-088607fcf1674831b4d0ede632494377
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652047B2

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