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

HRID 380582ノート

反応式

HRID 380582 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-53432d1912f3475fb60152b86f1bd868
出典データセット
uspto-grants-2001_10
特許番号
US06303636B1

反応ノート

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