Reaktion #160412

ord-224f84fba2b94cfab3920299c0ab9252

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with DCM (2×15 mL)
  2. 2
    TemperaturThe basic aqueous layer was cooled in an ice bath
  3. 3
    ExtraktionThe acidic aqueous layer was extracted with DCM (3×20 mL)
  4. 4
    WaschenThe combined organic extracts were washed with brine
  5. 5
    Trocknendried over Na2SO4
  6. 6
    Filtrationfiltered

Vorschrift

To a solution of 3.47 g (13.2 mmol) of 2-cyclohexanesulfonyl-2-methyl-propionic acid ethyl ester in THF/water (4/1, 50 mL) were added 1.11 g (26.4 mmol) of lithium hydroxide monohydrate. The reaction was stirred at room temperature for 18 h. The reaction was further diluted with water (20 mL) and then washed with DCM (2×15 mL). The basic aqueous layer was cooled in an ice bath and then acidified with 1M aqueous HCl solution to pH 2. The acidic aqueous layer was extracted with DCM (3×20 mL). The combined organic extracts were washed with brine, dried over Na2SO4 and filtered. Concentration of the filtrate under reduced pressure afforded 2.96 g of 2-cyclohexanesulfonyl-2-methyl-propionic acid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829034B2uspto-grants-2014_09