تفاعل #8774

ord-f27a956677fb4f649e90173553ade153

المذيبات

ظروف التفاعل

درجة الحرارة
75°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 (0.250 g, 0.77 mmol), potassium carbonate (0.22 g, 1.59 mmol), 4-methylpiperidine (0.382 g, 3.85 mmol) and acetonitrile (4.0 mL) and heat at 75° 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 dichloromethane to 10% methanol in dichloromethane to obtain the title compound (0.254 g, 96% Yield) as an amber oil. Purity by LC/MS (APCI)=99%, [M+H]+=343.

المصدر

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