Nitromethane → HCID 66692011, Verbindung

HRID 2041108Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2041108
[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=O.[N+:12]([CH3:15])([O-:14])=[O:13].C([O-])(=O)C.[NH4+]>C(O)(=O)C>[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[CH:15][N+:12]([O-:14])=[O:13]

Komponenten

5

Edukt 3

HCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 27348722-Fluoro-5-methoxybenzaldehyde

Produkt 1

HCID 66692011HCID 66692011, VerbindungAusbeute 97,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Heat 2-fluoro-5-methoxybenzaldehyde (15 g, 97.4 mmol) with nitromethane (32 mL, 584 mmol) and ammonium acetate (30 g, 390 mmol) in acetic acid (136 mL) under reflux for 30 min. Evaporate the solvent and dissolve the residue in ether. Wash the organic fraction with water, saturated aqueous NaHCO3 and evaporate to give the desired intermediate (18.7 g, 97%). GC-MS m/z: 197 (M)+.

Aufarbeitung

  1. temperatureunder reflux for 30 min
  2. customEvaporate the solvent
  3. dissolutiondissolve the residue in ether
  4. washWash the organic fraction with water, saturated aqueous NaHCO3
  5. customevaporate

Quellen und Nachweise

ORD-Eintrag
ord-ffb1f75d75994092939b37275cd9e508
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08580780B2

Notizen zur Reaktion

Wird geladen…