تفاعل #521398

ord-27427512053c4a09b794d01d097195cb

المذيبات

ظروف التفاعل

درجة الحرارة
30°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحFor work-up, the solid is filtered off with suction
  2. 2
    workup.ADDITIONthe filtrate is diluted with methylene chloride
  3. 3
    استخلاصextracted with water
  4. 4
    غسيلwashed twice with water
  5. 5
    أخرىThe organic phase is dried
  6. 6
    تركيزconcentrated

الإجراء التجريبي

30 g (170 mmol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline are dissolved in 400 ml of acetonitrile, and 94 g (0.68 mol) of potassium carbonate are added. 84 g (174 mmol) of tetrabutylammonium tribromide are subsequently added a little at a time with vigorous stirring at temperatures<30° C. For work-up, the solid is filtered off with suction and the filtrate is diluted with methylene chloride and extracted with water. The solvent is stripped off and the residue is again taken up in methyl tert-butyl ether and washed twice with water. The organic phase is dried and concentrated.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06670482B2uspto-grants-2003_12