تفاعل #2139954

ord-8effeacce2064b4d81a75da8ac834529

معادلة التفاعل

CCOc1ccc(Br)c(C(=O)Oc2c(Br)ccc(OCc3ccccc3)c2F)c1F
3-benzyloxy-6-bromo-2-fluorophenyl 6-bromo-3-ethoxy-2-fluorobenzoate
CCOc1ccc2c(c1F)c(=O)oc1c(F)c(OCc3ccccc3)ccc12
8-ethoxy-4,7-difluoro-3-benzyloxybenzo[c]chromen-6-one
المردود 21.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ethyl acetate
  2. 2
    تجفيفthe combined extracts were dried over sodium sulfate
  3. 3
    أخرىevaporated
  4. 4
    أخرىCrystallisation of the crude product from THF

الإجراء التجريبي

103 g (0.188 mol) of 3-benzyloxy-6-bromo-2-fluorophenyl 6-bromo-3-ethoxy-2-fluorobenzoate were dissolved in 1 l of DMF and refluxed for 72 hours in the presence of 119 g (1.88 mol) of copper powder. The batch was subsequently diluted with water and extracted with ethyl acetate, and the combined extracts were dried over sodium sulfate and evaporated. Crystallisation of the crude product from THF gave 15 g (21% of theory) of 8-ethoxy-4,7-difluoro-3-benzyloxybenzo[c]chromen-6-one as pale-yellow crystals.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07326447B2uspto-grants-2008_02