Hydrochloric Acid → Ethyl 3-acetylamino-2-nitrobenzoate

HRID 276027Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 276027
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[C:7]([N+:17]([O-:19])=[O:18])=[C:8]([CH:14]=[CH:15][CH:16]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10].Cl>CN(C)C1C=CC=CC=1>[C:1]([NH:5][C:6]1[C:7]([N+:17]([O-:19])=[O:18])=[C:8]([CH:14]=[CH:15][CH:16]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 18315537Ethyl 3-amino-2-nitrobenzoate

Produkt 1

HCID 18315582Ethyl 3-acetylamino-2-nitrobenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 949N,N-DimethylanilineLösungsmittel

Versuchsvorschrift

Acetyl chloride (13 ml) was added dropwise to a solution of 2.98 g of ethyl 3-amino-2-nitrobenzoate and 20 ml of N,N-dimethylaniline in an ice bath. The mixture was stirred at room temperature for 48 hours. The reaction solution was acidified with 10% hydrochloric acid, and was extracted twice with ethyl acetate. The organic layer was washed three times with water. The solvent was distilled off under reduced pressure, and the resulting residue was crystallized with hexane. The crystals were separated through filtration, washed with hexane, and dried to give 3.30 g of ethyl 3-acetylamino-2-nitrobenzoate.

Aufarbeitung

  1. extractionwas extracted twice with ethyl acetate
  2. washThe organic layer was washed three times with water
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe resulting residue was crystallized with hexane
  5. customThe crystals were separated through filtration
  6. washwashed with hexane
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7a01beb7110244ddb1150a9f6048d994
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06352985B1

Notizen zur Reaktion

Wird geladen…