تفاعل #85807

ord-cc1fb27aad36408cadc3dd063474605a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux overnight
  2. 2
    تركيزThe mixture was concentrated
  3. 3
    workup.ADDITIONdiluted with water
  4. 4
    استخلاصextracted with EtOAc
  5. 5
    تجفيفThe combined extracts were dried over Na2SO4
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated
  8. 8
    أخرىThe residue was purified by preparative thin-layer chromatography

الإجراء التجريبي

A solution of 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzenamine (164 mg, 0.75 mmol), 1-bromo-2-(2-bromoethoxy)ethane (418 mg, 1.8 mmol), and DIPEA (0.64 mL, 3.6 mmol) in THF (2 mL) was stirred at reflux overnight. The mixture was concentrated, diluted with water, and extracted with EtOAc. The combined extracts were dried over Na2SO4, filtered, and concentrated. The residue was purified by preparative thin-layer chromatography to give the title compound. MS (m/z): 290 (M+H)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434726B2uspto-grants-2016_09