تفاعل #73969

ord-199563e105234712aa9009e8a9abcee2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe reaction mixture was extracted with DCM (2×25 mL)
  2. 2
    غسيلThe combined orgaic layers were washed with water (10 mL), brine (10 mL)
  3. 3
    تجفيفdried (Na2SO4)
  4. 4
    تركيزconcentrated
  5. 5
    أخرىThe crude material was purified by flash chromatography on silica gel eluting with 50% EtOAc in DCM

الإجراء التجريبي

To a solution of (E)-ethyl 3-(4-(4-(chlorosulfonyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate (intermediate 41.3) (250 mg, 0.60 mmol) in DCM (3 mL) was added a solution of 2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethanamine (157 mg, 0.72 mmol) and triethylamine (72 mg, 0.72 mmol) in DCM (2 mL). After 15 minutes, water (10 mL) was added and the reaction mixture was extracted with DCM (2×25 mL). The combined orgaic layers were washed with water (10 mL), brine (10 mL), dried (Na2SO4) and concentrated. The crude material was purified by flash chromatography on silica gel eluting with 50% EtOAc in DCM to give the title compound (169 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541448B2uspto-grants-2013_09