Reaktion #334449

Reaktionsgleichung

sodium hypochlorite

sodium hydroxide

2-hydroxy-6-methylnicotinic acid

→

5-Chloro-2-hydroxy-6-methyl-3-pyridinecarboxylic acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONWhen the acid had dissolved
2. 2
   FiltrationThe reaction mixture was then filtered
3. 3
   SonstigeThe precipitate was recrystallized from isopropyl alcohol/ethereal
4. 4
   Sonstigeto give ~6 g of analytically pure crystals, m.p. 291°-94° C.

Vorschrift

To a solution of 15.7 g of 50% sodium hydroxide and 18.2 ml of water was added 10 g (0.065 mole) of 2-hydroxy-6-methylnicotinic acid. When the acid had dissolved, 200 ml of 5.25% aqueous sodium hypochlorite was added rapidly through a dropping funnel. The temperature was not moderated (slight exotherm did occur). The entire mixture was stirred at room temperature for 18 hr. The reaction mixture was then filtered and acidified with concentrated hydrochloric acid. The precipitate was recrystallized from isopropyl alcohol/ethereal to give ~6 g of analytically pure crystals, m.p. 291°-94° C.

Quelle