Reaktion #656273

Reaktionsgleichung

3-cyano-2-oxo-8-chromenyloxyacetic acid methyl ester

tetrahydrothiophene

aluminium bromide

hydrochloric acid

→

desired compound

3-cyano-2-oxo-8-chromenyloxyacetic acid

Lösungsmittel

methyl chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas gradually added
2. 2
   Sonstigewas brought to room temperature
3. 3
   workup.ADDITIONwas gradually added
4. 4
   workup.STIRRINGAfter stirring for 2 hours
5. 5
   Filtrationa precipitate was filtered
6. 6
   Sonstigewhich was recrystallized

Vorschrift

Ten ml of tetrahydrothiophene was cooled with ice, to which 13.4 g of pulverized anhydrous aluminium bromide was gradually added. After stirring for 5 minutes, a temperature was brought to room temperature and then a solution of 2.6 g of 3-cyano-2-oxo-8-chromenyloxyacetic acid methyl ester dissolved in 30 ml of methyl chloride was gradually added. After stirring for 2 hours, the reaction mixture was poured into a mixture of 20 ml of concentrated hydrochloric acid and 200 ml of ice water and a precipitate was filtered, which was recrystallized to give a desired compound.

Quelle