반응 #2205

ord-5e3cc0d24c92424b96fce5ec22cba17e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONof p-toluenesulfonic add
  2. 2
    기타was evaporated
  3. 3
    workup.ADDITIONthe residue was poured into 200 ml of water
  4. 4
    추출The aqueous solution was extracted with hexane (2×100 ml)
  5. 5
    추출re-extracted with ether (3×100 ml)
  6. 6
    세척The combined ether extracts were washed with 100 ml of brine
  7. 7
    건조dried over magnesium sulfate
  8. 8
    기타evaporated

실험 절차

To a mixture of 5.0 g of 2-butyne-1,4-diol and 10 milligrams of p-toluenesulfonic add and 150 ml of dry ether there was added dropwise with stirring at room temperature 4.9 g of 3,4-dihydro-2H-pyran. After stirring overnight at ambient temperature the ether was evaporated and the residue was poured into 200 ml of water. The aqueous solution was extracted with hexane (2×100 ml) and then re-extracted with ether (3×100 ml). The combined ether extracts were washed with 100 ml of brine, dried over magnesium sulfate and evaporated to yield 6.8 g of 4-tetrahydropyranoxy-2-butyn-1-ol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728698uspto-grants-1998_03