1,2-Dichloroethane → HCID 22326844, Verbindung

HRID 495455Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 495455
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:4]=1[CH2:12][C:13]([OH:15])=O.C(Cl)CCl.C[CH2:21][N:22](CC)[CH2:23]C.Cl.CNC>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:4]=1[CH2:12][C:13]([N:22]([CH3:23])[CH3:21])=[O:15]

Komponenten

6

Edukt 4

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 35192982-(2-methoxy-5-nitrophenyl)acetic acid

Produkt 1

HCID 22326844HCID 22326844, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

2-(2-Methoxy-5-nitrophenyl)acetic acid (17.1 g, 1 eq, Step B), EDC (18.6 g, 1.2 eq.), Et3N (9.8 g, 13.6 mL, 1.2 eq) and dimethylamine hydrochloride (7.9 g, 1.2 eq.) in 150 mL of CH2Cl2 were stirred together with exclusion of air overnight. CH2Cl2 (150 mL) was added and the mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine. Removal of the solvent under reduced pressure followed by silica gel chromatography (90:10 CH2Cl2:EtOAc) afforded pure 2-(2-methoxy-5-nitrophenyl)-N,N-dimethyl-acetamide as a white solid.

Aufarbeitung

  1. washthe mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine
  2. customRemoval of the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a6595046bb5b4d8dbbd4426b89f2d4ff
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06939874B2

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