反应 #2139954

ord-8effeacce2064b4d81a75da8ac834529

反应方程式

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
收率 21.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with ethyl acetate
  2. 2
    干燥the combined extracts were dried over sodium sulfate
  3. 3
    其他evaporated
  4. 4
    其他Crystallisation of the crude product from THF

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07326447B2uspto-grants-2008_02