تفاعل #6686

ord-ed18f3b23e5b4b238c3b0edae8dd78e6

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىquenched with water
  2. 2
    استخلاصextracted with ethyl acetate:hexane (1:1)
  3. 3
    غسيلwashed with brine
  4. 4
    تجفيفdried over MgSO4
  5. 5
    تركيزconcentrated in vacuo
  6. 6
    أخرىPurification by chromatography
  7. 7
    أخرىon silica gel (5% EtOAc/hexanes) and recrystallization from acetonitrile

الإجراء التجريبي

Sodium hydride (1 equi.) was added to the solution of 4-(2,3-difluorophenoxy)-butan-1-ol (22), (1 equi.) and 1-bromopentane (1 equi.) in DMF (1 mL/mmole) and the reaction mixture was stirred at room temperature for 12 h,. quenched with water, extracted with ethyl acetate:hexane (1:1), washed with brine, dried over MgSO4, and concentrated in vacuo. Purification by chromatography on silica gel (5% EtOAc/hexanes) and recrystallization from acetonitrile gave 1,2-difluoro-3-(4-pentyloxybutoxy)-benzene (24), as a white solid (84%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07083832B2uspto-grants-2006_08