반응 #9565

ord-5574c035cb5d4caf8df4dacdca15baab

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe reaction was stirred for four additional days
  2. 2
    기타The methanol was removed under reduced pressure
  3. 3
    workup.ADDITIONSolid sodium chloride was added to the aqueous layer, which
  4. 4
    추출was extracted with chloroform (3×150 mL)
  5. 5
    건조The combined extracts were dried over sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated under reduced pressure

실험 절차

Ammonium hydroxide (1 L) was added to a solution of methyl tetrahydro-2H-pyran-4-carboxylate (20 mL, 150 mmol) in methanol (500 mL), and the reaction was stirred overnight at ambient temperature. Additional ammonium hydroxide (500 mL) was added, and the reaction was stirred for four additional days. The methanol was removed under reduced pressure. Solid sodium chloride was added to the aqueous layer, which was extracted with chloroform (3×150 mL). The combined extracts were dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide 11.4 g of tetrahydropyran-4-carboxamide as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08