Reaktion #572247

Reaktionsgleichung

4-Picolylacetate

hydrobromic acid

→

4-picolylbromide hydrobromide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigerising from 26° to 42° C
2. 2
   TemperaturThe mixture was heated
3. 3
   Temperaturto reflux
4. 4
   EinengenThe reaction mixture was then concentrated in vacuo
5. 5
   Sonstigeto yield a gummy solid which
6. 6
   workup.DISSOLUTIONwas dissolved in 1500 ml
7. 7
   SonstigeCrude hydrobromide salt (379 g.) crystallized
8. 8
   Temperaturon chilling
9. 9
   Filtrationwas recovered by filtration

Vorschrift

4-Picolylacetate (300 g., 87% pure) was combined with 3.0 l. of 48% hydrobromic acid. A spontaneous exotherm occurred, the temperature rising from 26° to 42° C. The mixture was heated to reflux and refluxed for about 1 hour (pot temperature 124° C.). The reaction mixture was then concentrated in vacuo to yield a gummy solid which was dissolved in 1500 ml. of absolute alcohol. Crude hydrobromide salt (379 g.) crystallized on chilling and was recovered by filtration. Purified 4-picolylbromide hydrobromide (33.1 g., m.p. 187.5°-189° C.) was obtained by recrystallization of 50 g. of crude from absolute alcohol.

Quelle