反応 #340704

ord-524ac23436b4475b829b14ad4d818060

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to separate
  2. 2
    洗浄washed with water and brine
  3. 3
    乾燥dried with anhydrous sodium sulfate (Na2SO4)
  4. 4
    その他After rotary evaporation
  5. 5
    その他to remove the solvent

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07872046B2uspto-grants-2011_01