تفاعل #8769

ord-4538b46408a348e9ba852736e080caa3

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةCool the reaction mixture
  2. 2
    ترشيحfilter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate)
  3. 3
    تركيزCombine the appropriate fractions and concentrate
  4. 4
    أخرىto give a residue
  5. 5
    أخرىPurify the residue by column (10 g silica) chromatography

الإجراء التجريبي

Mix 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole (0.40 g, 1.23 mmol), potassium carbonate (0.341 g, 2.47 mmol), 2-fluorobenzylamine (0.626 g, 5.0 mmol) and acetonitrile (5.0 mL) and heat at 80° C., overnight. Cool the reaction mixture and filter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate). Combine the appropriate fractions and concentrate to give a residue. Purify the residue by column (10 g silica) chromatography using a solvent gradient of 40% ethyl acetate in heptane to 100% ethyl acetate to obtain the title compound (0.378 g, 83% Yield). Purity by LC/MS (APCI)=99%, [M+H]+=369.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091199B1uspto-grants-2006_08