تفاعل #2332018

ord-92890d6f913a42d7ac51efd2a663901f

معادلة التفاعل

C#CC(CCCCC)Oc1cccc(F)c1F
1-(1-ethynylhexyloxy)-2,3-difluorobenzene
CCCCCC1C=Cc2ccc(F)c(F)c2O1
7,8-difluoro-2-pentyl-2H-chromene

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed a number of times with 1 N HCl
  2. 2
    أخرىThe organic phase is dried
  3. 3
    تركيزconcentrated to dryness
  4. 4
    أخرىThe residue is purified by column chromatography (SiO2, n-pentane:1-chlorobutane=5:1)

الإجراء التجريبي

62.0 g (0.26 mol) of 1-(1-ethynylhexyloxy)-2,3-difluorobenzene are heated at 195° C. for 2 h in 390 ml of N,N-diethylaniline. The batch is diluted with MTBE and washed a number of times with 1 N HCl. The organic phase is dried using sodium sulfate and concentrated to dryness. The residue is purified by column chromatography (SiO2, n-pentane:1-chlorobutane=5:1), giving 7,8-difluoro-2-pentyl-2H-chromene as a brown oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07678929B2uspto-grants-2010_03