Hydrochloric Acid → 3-Fluoro-4-nitrobenzyl alcohol

Temperatur

0 °C

To a solution of 3-fluoro-4-nitrobenzoic acid (2.0 g, 10.8 mmol) in THF (50 ml) at 0° C. was added BH3.Me2S complex (2.215 ml, 22.15 mmol) drop-wise. The mixture was stirred at 0° C. for 3 h, and was then stirred at 65° C. for 18 h. To the cooled mixture was added ice (50 g), followed by 1 N aq. HCl (100 ml), and the resulting mixture was extracted with EtOAc (200 ml). The organic layer was dried over Na2SO4, filtered and concentrated in vacuo to provide the title compound as a white solid (1.79 g, 97%).

1. stirringwas then stirred at 65° C. for 18 h
2. extractionthe resulting mixture was extracted with EtOAc (200 ml)
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo

ORD-Eintrag

ord-8f79d2b6447d4908af02191330167dde

Quelldatensatz

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08415351B2