Methanol → Methyl 2-chloro-6-methoxyisonicotinate

HRID 245078

Reaktionsgleichung

Reaktionsgleichung von HRID 245078
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:11][CH3:12])[N:10]=1)[C:5]([OH:7])=[O:6].[CH3:13]O>OS(O)(=O)=O>[CH3:13][O:6][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([O:11][CH3:12])[N:10]=[C:2]([Cl:1])[CH:3]=1

Komponenten

4

Edukt 2

HCID 887MethanolHCID 27821242-Chloro-6-methoxypyridine-4-carboxylic acid

Produkt 1

HCID 13339618Methyl 2-chloro-6-methoxyisonicotinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a suspension of 2-chloro-6-methoxy-isonicotinic acid (244 g, 1.30 mol) in methanol (2.5 L), H2SO4 (20 mL) is added. The mixture is stirred at reflux for 24 h before it is cooled to 0° C. The solid material is collected, washed with methanol (200 mL) and water (500 mL) and dried under HV to give 2-chloro-6-methoxy-isonicotinic acid methyl ester (165 g) as a white solid; LC-MS: tR=0.94 min, [M+1]+=201.89.

Aufarbeitung

  1. additionis added
  2. temperatureat reflux for 24 h before it
  3. customThe solid material is collected
  4. washwashed with methanol (200 mL) and water (500 mL)
  5. customdried under HV

Quellen und Nachweise

ORD-Eintrag
ord-0a7cf0719f6146c0aaeb39853efd8457
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658675B2

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