반응 #77920

반응 방정식

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

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added to a reactor
2. 2
   온도The reaction mixture was cooled down to room temperature
3. 3
   기타Toluene layer separated
4. 4
   건조was dried over anhydrous MgSO4
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타to give crude product
8. 8
   기타The crude product was purified by column chromatograph on silica gel
9. 9
   세척by eluting with a mixture of ethylacetate and n-hexane (1:5)

실험 절차

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 % .

출처