تفاعل #77920

ord-1f4befc33ffa492db518647e07a976d7

المذيبات

ظروف التفاعل

درجة الحرارة
220°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added to a reactor
  2. 2
    درجة الحرارةThe reaction mixture was cooled down to room temperature
  3. 3
    أخرىToluene layer separated
  4. 4
    تجفيفwas dried over anhydrous MgSO4
  5. 5
    ترشيحfiltered
  6. 6
    أخرىevaporated
  7. 7
    أخرىto give crude product
  8. 8
    أخرىThe crude product was purified by column chromatograph on silica gel
  9. 9
    غسيلby eluting with a mixture of ethylacetate and n-hexane (1:5)

الإجراء التجريبي

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 % .

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06706917B1uspto-grants-2004_03