反応 #77920

反応方程式

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

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONwas added to a reactor
2. 2
   温度The reaction mixture was cooled down to room temperature
3. 3
   その他Toluene layer separated
4. 4
   乾燥was dried over anhydrous MgSO4
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   その他to give crude product
8. 8
   その他The crude product was purified by column chromatograph on silica gel
9. 9
   洗浄by eluting with a mixture of ethylacetate and n-hexane (1:5)

実験手順

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 % .

出典