تفاعل #1012602

ord-b5fe260349a5474e9f4705a320e64dca

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction mixture was stirred at the same temperature for 1.5 h
  2. 2
    استخلاصthe reaction mixture extracted with AcOEt (3×50 mL)
  3. 3
    تجفيفThe combined organic layers were dried over sodium sulfate
  4. 4
    أخرىafter removal of the solvent
  5. 5
    أخرىa solid was obtained
  6. 6
    أخرىwhich was triturated with hexane

الإجراء التجريبي

i-Propylmagnesium chloride (2 M in THF, 8.98 mL, 17.95 mmol) was added dropwise to a cooled (−30° C.) solution of 4-chloro-1-ethyl-2-iodobenzene (4.35 g, 16.3 mmol) in dry THF (40 mL) and the reaction mixture was stirred at the same temperature for 30 min, under argon. After this time, trimethylborate (3.63 mL, 32.6 mmol) was added dropwise and the reaction mixture was stirred at the same temperature for 1.5 h. HCl (1 M, 16 mL) was added and the reaction mixture extracted with AcOEt (3×50 mL). The combined organic layers were dried over sodium sulfate and, after removal of the solvent, a solid was obtained, which was triturated with hexane to obtain the title compound as a white solid (2.15 g, 72%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09284298B2uspto-grants-2016_03