تفاعل #9565

ord-5574c035cb5d4caf8df4dacdca15baab

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091214B2uspto-grants-2006_08