Water → 3-[[5-(Trifluoromethyl)-2-pyridyl]oxy]-1-propanamine

Temperatur

0 °C

2-Fluoro-5-trifluoromethylpyridine (1.831 g, 11 mmol) was dissolved in anhydrous THF (15 mL) with stirring under nitrogen and cooled to 0° C. in an ice bath. To this was added dropwise over 30 minutes a solution of 3-amino-1-propanol (0.76 mL, 10 mmol) in anhydrous THF (15 mL) and 1M potassium tert-butoxide in THF (10 mL, 10 mmol). The yellow solution was allowed to stir and warm to room temperature in the ice bath overnight. The reaction mixture was poured into water (75 mL) and extracted with ether (2×50 mL). The organic phase was washed with brine (50 mL), dried (Na2SO4), filtered and evaporated under vacuum to a yellow liquid, which was nearly pure by NMR and MS, and was used as such without further purification.

1. stirringto stir
2. extractionextracted with ether (2×50 mL)
3. washThe organic phase was washed with brine (50 mL)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated under vacuum to a yellow liquid, which
7. customsuch without further purification

ORD-Eintrag

ord-46fed52c4d99447b97b474bcc746b22f

Quelldatensatz

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06521622B1