Reaktion #340704

ord-524ac23436b4475b829b14ad4d818060

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto separate
  2. 2
    Waschenwashed with water and brine
  3. 3
    Trocknendried with anhydrous sodium sulfate (Na2SO4)
  4. 4
    SonstigeAfter rotary evaporation
  5. 5
    Sonstigeto remove the solvent

Vorschrift

To a stirred solution of 1-chloro-2-methylpropyl methylformate in dichloromethane (DCM) was added a solution of sodium methanethiolate (CH3—SNa) (1.0 eq.) in water at 0° C. and 0.02 eq. of tetrabutylammonium bromide. The reactants were stirred at 0° C. for 30 min and then diluted with dichloromethane (DCM). The dichloromethane layer was allowed to separate, then washed with water and brine, and dried with anhydrous sodium sulfate (Na2SO4). After rotary evaporation to remove the solvent, the title compound (6a) was obtained. 1H-NMR (CDCl3): δ 1.05 (d, J=5.6 Hz, 3H), 1.07 (d, J=5.6 Hz, 3H), 2.18 (m, 1H), 2.38 (s, 3H), 6.34 (d, J=5.6 Hz, 1H) ppm.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07872046B2uspto-grants-2011_01