Dimethylamine → 2-Dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridine

HRID 256163Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 256163
[OH:1][CH2:2][C:3]1[C:8]([F:9])=[C:7](F)[N:6]=[C:5]([F:11])[C:4]=1[F:12].[CH3:13][NH:14][CH3:15].O>C(O)C>[CH3:13][N:14]([CH3:15])[C:7]1[C:8]([F:9])=[C:3]([CH2:2][OH:1])[C:4]([F:12])=[C:5]([F:11])[N:6]=1

Komponenten

5

Edukt 3

HCID 674DimethylamineHCID 962WaterHCID 139851584-Hydroxymethyl-2,3,5,6-tetrafluoropyridine

Produkt 1

HCID 139851642-Dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridineAusbeute 87,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 1.0 g (0.0055 mole) of 4-hydroxymethyl-2,3,5,6-tetrafluoropyridine (from Example 5) and 0.23 g (0.0050 mole) of dimethylamine in 25 ml of ethanol was refluxed for approximately twenty hours. The reaction mixture was cooled and was poured into water. This mixture was extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated under reduced pressure, yielding 0.9 g of 2-dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridine as a yellow oil. The structure and nmr spectra are set forth in Table 1C below.

Aufarbeitung

  1. temperaturewas refluxed for approximately twenty hours
  2. temperatureThe reaction mixture was cooled
  3. extractionThis mixture was extracted with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-441e0d58445b4beaa592252f1f6fb227
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04701464

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