Methanesulfonyl chloride → [4-chloro-2-(1-chloroethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

HRID 38260Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 38260
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[C:4]([CH:17](O)[CH3:18])[CH:3]=1.CCN(C(C)C)C(C)C.CS([Cl:33])(=O)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[C:4]([CH:17]([Cl:33])[CH3:18])[CH:3]=1

Komponenten

5

Edukt 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 86631057[4-chloro-2-(1-hydroxyethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

Produkt 1

HCID 86631056[4-chloro-2-(1-chloroethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To the product of step b) (0.34 g) in DCM (5 ml) was added Hunigs base (1 ml) followed by methanesulfonyl chloride (0.46 ml) and the reaction stirred at room temperature for 2 h followed by heating at 45° C. for 2 h. After cooling to 0° C. the bulk of the volatiles were removed in vacuo. Diethyl ether and water were added and the organic layer separated.

Aufarbeitung

  1. temperatureby heating at 45° C. for 2 h
  2. temperatureAfter cooling to 0° C. the bulk of the volatiles
  3. customwere removed in vacuo
  4. additionDiethyl ether and water were added
  5. customthe organic layer separated

Quellen und Nachweise

ORD-Eintrag
ord-751bf4b766aa40ed99c35ebfb6283106
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524715B2

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