Water → Benzoic acid, 3-methoxy-2-nitro-, methyl ester

HRID 2206698

Reaktionsgleichung

Reaktionsgleichung von HRID 2206698
[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[C:15]([O-])([O-])=O.[K+].[K+].CI.O>CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:8][CH3:15])=[O:7]

Komponenten

6

Edukt 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 786323-Methoxy-2-nitrobenzoic acid

Produkt 1

HCID 79195Benzoic acid, 3-methoxy-2-nitro-, methyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a mixture of 3-methoxy-2-nitrobenzoic acid (25.0 g, 126 mmol) and K2CO3 (35.0 g, 253 mmol) in DMF (126 mL) was added MeI (15.8 mL, 253 mmol) at room temperature. The mixture was stirred at room temperature for 2 hours. To the mixture was poured the water (200 mL) and then stirred at 5° C. for 30 min. The precipitated solid was collected by filtration, washed with water and hexane. The solid was dried under reduced pressure to afford the compound 52 in a crude form (26.2 g, 98%) as a white solid.

Aufarbeitung

  1. stirringstirred at 5° C. for 30 min
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with water and hexane
  4. customThe solid was dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6acb2155199f4a66833f3c7de26e1609
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09371303B2

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