Diisopropylethylamine → HCID 86666020, Verbindung

To the solution of 2,7-dibromo-[1,2,4]triazolo[1,5-a]pyridine (5 g, 18.05 mmol) and (2-fluoro-ethyl)-methyl-amine hydrochloride (20 g, 180.5 mmol) in ethanol (30 ml) was added di-isopropylethylamine (47 ml, 270.75 mmol) and the reaction mixture was heated at 130° C. in a sealed tube for 84 hours. The reaction mixture was concentrated under reduced pressure, the resulting residue was diluted with dichloromethane (100 ml). The organic layer was washed with water (2×75 ml), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The crude material was purified by column chromatography over silicagel using 0.5% methanol/dichloromethane as eluent affording (7-bromo-[1,2,4]triazolo[1,5-a]pyridin-2-yl)-(2-fluoro-ethyl)-methyl-amine (1.7 g, 34.5%) as an off white solid. MS: m/z=275.2 (M+H+).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionthe resulting residue was diluted with dichloromethane (100 ml)
3. washThe organic layer was washed with water (2×75 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by column chromatography over silicagel

ORD-Eintrag

ord-bfb48cd994424fccbde0b66bcaacd411

Quelldatensatz

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08349824B2