Phosphorus pentachloride → 4-[(4-Fluorophenyl)methoxy]benzene-1-sulfonyl chloride

HRID 380582노트

반응식

HRID 380582 반응식
[F:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([S:14]([O-])(=[O:16])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Na+].P(Cl)(Cl)(Cl)(Cl)[Cl:22]>C(Cl)Cl>[F:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([S:14]([Cl:22])(=[O:16])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 23701365Sodium 4-(4-fluorobenzyloxy)benzenesulfonate

생성물 1

HCID 181794244-[(4-Fluorophenyl)methoxy]benzene-1-sulfonyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a slurry of sodium 4(4-fluorobenzyloxy)benzenesulfonate (0.5 grams, 1.64 mmole), in methylene chloride (5 mL) was added phosphorus pentachloride (275 mg, 1.31 mmole). The resulting mixture was heated at reflux for 7 hours. After cooling in an ice bath and quenching with water (15 mL), the mixture was extracted with ethyl acetate. The organic phase was washed brine, dried over sodium sulfate, and concentrated to afford 4-(4-fluorobenzyloxy)benzenesulfonyl chloride a white solid (130 mg, 26%).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 7 hours
  3. temperatureAfter cooling in an ice bath
  4. customquenching with water (15 mL)
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic phase was washed brine
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-53432d1912f3475fb60152b86f1bd868
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303636B1

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