Reaktion #11969

Reaktionsgleichung

compound

8-methylquinoline-5-carboxylic acid

methanol

hydrochloric acid

→

title compound

Methyl 8-methylquinoline-5-carboxylate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent was removed by distillation
2. 2
   workup.DISSOLUTIONThe obtained residue was dissolved in water
3. 3
   workup.ADDITION1 mol/l sodium hydroxide aqueous solution was added
4. 4
   Sonstigeto precipitate
5. 5
   FiltrationThe solid was collected by filtration
6. 6
   Extraktionthe filtrate was extracted with chloroform
7. 7
   TrocknenThe extract was dried over anhydrous sodium sulfate
8. 8
   Sonstigethe solvent was removed by distillation
9. 9
   Sonstigeto obtain a solid
10. 10
    Sonstigepurified by silica gel column chromatography (20 g, chloroform)

Vorschrift

The compound obtained in Example 87-2 (1 g) was dissolved in methanol (25 ml). The solution was stirred for 15 hours while blowing hydrochloric acid gas, and the solvent was removed by distillation. The obtained residue was dissolved in water and 1 mol/l sodium hydroxide aqueous solution was added to cause a solid substance to precipitate. The solid was collected by filtration and the filtrate was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was removed by distillation to obtain a solid. The solid was combined with the previously collected solid and purified by silica gel column chromatography (20 g, chloroform) to obtain the title compound (0.7337 g) as a white solid.

Quelle