1-Phenoxy-2-propanol → 1-Phenoxy-2-propyl methane sulfonate

HRID 1704733Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1704733
[O:1]([CH2:8][CH:9]([OH:11])[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:12](Cl)([OH:15])(=O)=[O:13].[CH4:17]>N1C=CC=CC=1>[CH3:17][S:12]([O:11][CH:9]([CH3:10])[CH2:8][O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)(=[O:15])=[O:13]

Komponenten

4

Edukt 2

HCID 928391-Phenoxy-2-propanolHCID 19821184HCID 19821184, Verbindung

Produkt 1

HCID 218874181-Phenoxy-2-propyl methane sulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

To 1-phenoxy-2-propanol (1 mole) dissolved in pyridine (500 ml) is added methane sulfochloride (1 mole) at a rate sufficient for the temperature of the reaction mixture to reach a value of 40°-50° C., with stirring. On completion of the addition, the reactor is sealed and the reaction mixture is left aside at room temperature during 48 hours. The reaction mixture is then poured over ice. The aqueous phase is extracted with methylene chloride. The organic phase is washed with dilute sulfuric acid and then with water to neutral pH. The resulting material is dried over sodium sulfate and concentrated, to give an oil which crystallizes. The material is taken up into ether, with stirring, to give a white precipitate which is suction filtered. M.p. = 58° C.

Aufarbeitung

  1. customa value of 40°-50° C.
  2. additionOn completion of the addition
  3. customthe reactor is sealed
  4. additionThe reaction mixture is then poured over ice
  5. extractionThe aqueous phase is extracted with methylene chloride
  6. washThe organic phase is washed with dilute sulfuric acid
  7. dry with materialThe resulting material is dried over sodium sulfate
  8. concentrationconcentrated
  9. customto give an oil which
  10. customcrystallizes
  11. stirringwith stirring
  12. customto give a white precipitate which
  13. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-0d2eef2c9fd2437392311485c6a0c531
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04127661

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