Reaktion #77920

Reaktionsgleichung

hydrochloric acid

Toluene

7-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone

acetic acid potassium salt

→

desired product

α-Methyl-3(2-naphthoyl)benzene Acetic Acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added to a reactor
2. 2
   TemperaturThe reaction mixture was cooled down to room temperature
3. 3
   SonstigeToluene layer separated
4. 4
   Trocknenwas dried over anhydrous MgSO4
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated
7. 7
   Sonstigeto give crude product
8. 8
   SonstigeThe crude product was purified by column chromatograph on silica gel
9. 9
   Waschenby eluting with a mixture of ethylacetate and n-hexane (1:5)

Vorschrift

A mixture of 7-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone (10 g) and acetic acid potassium salt (0.3 g) was added to a reactor and stirred for 1 hr at 220° C. The reaction mixture was cooled down to room temperature. Toluene and water were added to the reaction mixture and acidified to pH 2 with 5% hydrochloric acid. Toluene layer separated was dried over anhydrous MgSO4, filtered and evaporated to give crude product. The crude product was purified by column chromatograph on silica gel by eluting with a mixture of ethylacetate and n-hexane (1:5) to give the desired product (9:42 g, 94 % .

Quelle