반응 #733747

ord-bdc25266d2b84feeabcd22c105de5602

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe mixture was poured onto water
  2. 2
    추출extracted twice with diethyl ether
  3. 3
    세척The diethyl ether extracts were washed with water and brine
  4. 4
    건조dried over magnesium sulfate
  5. 5
    여과filtered
  6. 6
    기타evaporated
  7. 7
    기타to yield a yellow oil
  8. 8
    기타The oil was purified by column chromatography
  9. 9
    세척eluting with dichloromethane

실험 절차

1-Ethylsulfanyl-2-methyl-but-3-yn-2-ol (0.29 g, 2.0 mmol) was added to a mixture of sodium hydride (60% dispersion in mineral oil, 88 mg, 2.2 mmol) in dimethylformamide (5 mL) under argon. Iodomethane (0.12 mL, 2.0 mmol) was then added to the reaction mixture via syringe and the mixture allowed to stir overnight. The mixture was poured onto water and extracted twice with diethyl ether. The diethyl ether extracts were washed with water and brine, dried over magnesium sulfate, filtered, and evaporated to yield a yellow oil. The oil was purified by column chromatography eluting with dichloromethane to yield the title compound as a clear liquid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07705147B2uspto-grants-2010_04