Hydrochloric Acid → 3-Fluoro-4-nitrobenzyl alcohol

HRID 508376

Reaktionsgleichung

Reaktionsgleichung von HRID 508376
[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-9794bab93f224841acc2508a91c884a6
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09095590B2

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