Hydrochloric Acid → HCID 67970562, Verbindung

HRID 241439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 241439
[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 MeOH (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% yield). ES/MS (m/z) 216 (M+1).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-072d06f217394903b25797486c687845
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08648200B2

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