반응 #92974

ord-b2127b1f4ab840e882049e1d93516030

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was refluxed gently overnight
  2. 2
    추출The reaction mixture was extracted with 1 liter of isopropyl ether
  3. 3
    건조dried over sodium sulfate
  4. 4
    workup.DISTILLATIONdistilled under reduced pressure
  5. 5
    workup.DISTILLATIONThe distillate which was collected at 136°-138° C./0.015 mm

실험 절차

To a mixture of 2 moles (248.26 g.) of 2-methoxyphenol, 4 moles (160 g.) of sodium hydroxide, 250 ml. of water and 1 liter of isopropanol was added with stirring 2.2 moles (314.64 g.) of 1,4-dichloro-2-butanol. The mixture was refluxed gently overnight. The reaction mixture was extracted with 1 liter of isopropyl ether, dried over sodium sulfate and distilled under reduced pressure. The distillate which was collected at 136°-138° C./0.015 mm. (396.8 g.) solidified to a white crystalline solid which melted at 48°-50° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04609735uspto-grants-1986_09