تفاعل #3870

ord-62c89f061fa24da181f2e8c2e39d52b5

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe solution refluxed for 3 hours
  2. 2
    workup.ADDITIONThe reaction mixture is poured
  3. 3
    أخرىThe alkaline reaction mixture
  4. 4
    استخلاصis extracted with methylene chloride
  5. 5
    غسيلthe organic phase washed with water
  6. 6
    أخرىdried
  7. 7
    ترشيحfiltered
  8. 8
    أخرىevaporated in vacuo
  9. 9
    أخرىThe residue is chromatographed on silica gel eluting with ethyl acetate/hexane (1:3)

الإجراء التجريبي

7-Methoxy-3-piperidino-2,2-dimethylbenzofuran (65.1 g) is added to a stirred mixture of glacial acetic acid (340 ml) and 48% HBr (340 ml) and the solution refluxed for 3 hours. The reaction mixture is poured into crushed ice/H2O and brought to a pH=8-10. The alkaline reaction mixture is extracted with methylene chloride and the organic phase washed with water, dried, filtered and evaporated in vacuo. The residue is chromatographed on silica gel eluting with ethyl acetate/hexane (1:3) affording the desired product as a liquid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04722925uspto-grants-1988_02