Reaktion #1473412

Reaktionsgleichung

phloroglucinol dihydrate

ethyl 2-benzylacetoacetate

HCl

→

3-Benzyl-5,7-dihydroxy-4-methyl-2H-1-benzopyran-2-one

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas kept at that temperature overnight
2. 2
   EinengenThe yellow solution was concentrated
3. 3
   Sonstigetriturated with water
4. 4
   Filtrationthe solids filtered
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried
7. 7
   Sonstigeevaporated to dryness from toluene
8. 8
   Sonstigetriturated with petroleum ether (bp. 40-60° C.)
9. 9
   Filtrationfiltered

Vorschrift

A solution of phloroglucinol dihydrate (20 g) and ethyl 2-benzylacetoacetate (27.5 ml) in ethanol (320 ml) was treated with dry HCl at 0° C. for five hours and the solution was kept at that temperature overnight. The yellow solution was concentrated and triturated with water, the solids filtered, washed with water and dried. The resulting hydrate was thrice evaporated to dryness from toluene, triturated with petroleum ether (bp. 40-60° C.) and filtered. Yield 33,4 g (96%). Melting point 258-260° C.

Quelle