تفاعل #80271

ord-b85621a70dcc4cf1a64757f4dd2df935

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    أخرىwas returned to room temperature
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with water
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    تركيزThen, it was concentrated under reduced pressure
  7. 7
    أخرىthe oily substance thereby obtained
  8. 8
    أخرىwas purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1)

الإجراء التجريبي

A mixture comprising 2.1 g of 4-formyl-5-hydroxy-3-methylbenzothiophene, 2.4 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1.8 g of potassium carbonate in 30 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for 3 hours. The mixture was returned to room temperature, then poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Then, it was concentrated under reduced pressure, and the oily substance thereby obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1) to obtain 3.1 g (yield: 86%) of the desired compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05616537uspto-grants-1997_04