2,4-Dimethoxybenzylamine → N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine

HRID 537027

Reaktionsgleichung

Reaktionsgleichung von HRID 537027
F[C:2]1[CH:7]=[C:6]([I:8])[C:5]([CH3:9])=[CH:4][N:3]=1.[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=1[CH2:20][NH2:21]>CCOC(C)=O>[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=1[CH2:20][NH:21][C:2]1[CH:7]=[C:6]([I:8])[C:5]([CH3:9])=[CH:4][N:3]=1

Komponenten

4

Edukt 2

HCID 5972502,4-DimethoxybenzylamineHCID 100600522-Fluoro-4-iodo-5-methylpyridine

Produkt 1

HCID 66747638N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amineAusbeute 57 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A mixture of 2-fluoro-4-iodo-5-methylpyridine (60 g, 253 mmol) and 1-(2,4-dimethoxyphenyl)methanamine (190.6 mL, 1270 mmol) was allowed to stir at 110° C. overnight. The mixture was allowed to cool to rt and was then diluted with EtOAc (190 mL). The resulting solid was filtered and washed with EtOAc and then purified by column chromatography to give N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine (55.0 g, 57%).

Aufarbeitung

  1. temperatureto cool to rt
  2. filtrationThe resulting solid was filtered
  3. washwashed with EtOAc
  4. custompurified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-325d4bda78d84a6fa902d9be0996752d
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08859768B2

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