Reaktion #9565

Reaktionsgleichung

Ammonium hydroxide

methyl tetrahydro-2H-pyran-4-carboxylate

ammonium hydroxide

→

tetrahydropyran-4-carboxamide

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle