N-methyl-2-pyrrolidone → 2-Amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine

HRID 610187Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 610187
CN1CCCC1=O.[NH2:8][C:9]1[C:14]([F:15])=[C:13]([CH3:16])[C:12]([F:17])=[C:11](F)[N:10]=1.[CH3:19][O:20][C:21]1[CH:28]=[CH:27][C:24]([CH2:25][NH2:26])=[CH:23][CH:22]=1>C(Cl)(Cl)Cl>[NH2:8][C:9]1[C:14]([F:15])=[C:13]([CH3:16])[C:12]([F:17])=[C:11]([NH:26][CH2:25][C:24]2[CH:27]=[CH:28][C:21]([O:20][CH3:19])=[CH:22][CH:23]=2)[N:10]=1

Komponenten

5

Edukt 3

HCID 13387N-methyl-2-pyrrolidoneHCID 754524-MethoxybenzylamineHCID 125080923,5,6-Trifluoro-4-methylpyridin-2-amine

Produkt 1

HCID 221212712-Amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridineAusbeute 38,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

To 3 ml of N-methylpyrrolidone were added 1.35 g of 2-amino-3,5,6-trifluoro-4-methylpyridine together with 3.0 g of p-methoxybenzylamine, and the mixture was stirred under nitrogen atmosphere at 140° C. for 18 hours and allowed to cool. After adding 30 ml of chloroform, the mixture was washed three times with 300 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to chromatography (silica gel, 20 g; eluent: chloroform:n-hexane, 1:1, and then, chloroform) to obtain 0.90 g of the title compound as a pale yellow crude oil.

Aufarbeitung

  1. temperatureto cool
  2. washthe mixture was washed three times with 300 ml of distilled water
  3. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9354dd18568e427eab68de0ce01ea9a4
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US05998436

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