Hydrochloric Acid → HCID 67970562, Verbindung

HRID 889535Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889535
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH:13]([F:15])[F:14])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:2].[ClH:16].[H][H]>[Pd].CO>[ClH:16].[NH2:2][CH2:1][C:3]1[CH:4]=[CH:5][C:6]([CH:13]([F:14])[F:15])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 67970696HCID 67970696, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 67970562HCID 67970562, VerbindungAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

Purge a mixture of methyl 5-cyano-2-(difluoromethyl)benzoate (9.37 g, 44.4 mmol, 1.0 equiv), palladium (10% on carbon, 3.00 g, 2.82 mmol, 0.064 equiv), and methanol (50 mL) with nitrogen, then add hydrochloric acid (37 wt % aqueous, 8.0 mL, 105.6 mmol, 2.38 equiv), and stir the resulting suspension under 275 kPaG of hydrogen at room temperature overnight. Remove the solids by filtration, concentrate the filtrate under reduced pressure, and dry the resulting material in a 40° C. vacuum oven overnight to give the title compound as a light brown solid (7.01 g, 83%). MS (m/z) 216 (M+1).

Aufarbeitung

  1. customPurge
  2. customRemove the solids
  3. filtrationby filtration
  4. concentrationconcentrate the filtrate under reduced pressure
  5. customdry the resulting material in a 40° C. vacuum oven overnight

Quellen und Nachweise

ORD-Eintrag
ord-d81194d3ad3445abae548a18128aa598
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252831B2

Notizen zur Reaktion

Wird geladen…