Hydrochloric Acid → 3-Fluoro-4-nitrobenzyl alcohol

HRID 876127

Reaktionsgleichung

Reaktionsgleichung von HRID 876127
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5](O)=[O:6].Cl>C1COCC1>[F:1][C:2]1[CH:3]=[C:4]([CH2:5][OH:6])[CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12]

Komponenten

4

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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%).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-973d2c5a10ab4047acd96d5dc5766260
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08986740B2

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