Triethylamine → 3-(2-Chloro-4-trifluoromethoxyphenoxy)propyl methane sulfonate

HRID 229351Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 229351
[Cl:1][C:2]1[CH:12]=[C:11]([O:13][C:14]([F:17])([F:16])[F:15])[CH:10]=[CH:9][C:3]=1[O:4][CH2:5][CH2:6][CH2:7][OH:8].[CH3:18][S:19](Cl)(=[O:21])=[O:20].C(N(CC)CC)C>ClCCl>[CH3:18][S:19]([O:8][CH2:7][CH2:6][CH2:5][O:4][C:3]1[CH:9]=[CH:10][C:11]([O:13][C:14]([F:16])([F:15])[F:17])=[CH:12][C:2]=1[Cl:1])(=[O:21])=[O:20]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 685273763-(2-Chloro-4-trifluoromethoxyphenoxy)propanol

Produkt 1

HCID 865928333-(2-Chloro-4-trifluoromethoxyphenoxy)propyl methane sulfonateAusbeute 98,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 3-(2-chloro-4-trifluoromethoxyphenoxy)-propanol (20 g, 0.074 mole) in 100 mL of dichloromethane at 0° C. was added methanesulfonyl chloride (6.83 mL, 0.089 mole) and triethylamine (20.5 mL, 0.148 mole). The resulting solution was stored in a refrigerator overnight. The solution was then washed with 100 mL of cooled, diluted HCl-H2O solution. The organic layer was separated, dried over MgSO4, filtered and evaporated of solvent to yield 25.4 g of the product.

Aufarbeitung

  1. customwas stored in a refrigerator overnight
  2. washThe solution was then washed with 100 mL
  3. temperatureof cooled
  4. customThe organic layer was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated of solvent

Quellen und Nachweise

ORD-Eintrag
ord-4770e3ef45524b14bf0d3d98a853c310
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563792B2

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