تفاعل #156299

ord-7a16a80309be49a386bd3f3d8860fd8b

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصfollowed by extraction with ethyl acetate
  2. 2
    غسيلThe organic layer was washed with saturated brine
  3. 3
    تجفيفdried over anhydrous magnesium sulfate
  4. 4
    أخرىThe solvent was evaporated under reduced pressure
  5. 5
    أخرىthe residue was purified by silica gel column chromatography (chloroform/methanol)

الإجراء التجريبي

A mixture of 3 g of 4-ethoxybutyl p-toluenesulfonate, 2.65 g of tert-butyl (3R)-3-methylpiperazine-1-carboxylate, 3.07 mL of triethylamine, and 30 mL of acetonitrile was stirred at 90° C. for 3 hours. The reaction mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 3.1 g of tert-butyl (3R)-4-(4-ethoxybutyl)-3-methylpiperazine-1-carboxylate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822448B2uspto-grants-2014_09