تفاعل #63214

ord-041fa8d9cec1462ca5db313f84321533

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in ethanol
  3. 3
    workup.ADDITIONthe solution was treated with an equimolar amount of ethanolic hydrochloric acid
  4. 4
    أخرىThe hydrochloride was recrystallized from methanol/ether

الإجراء التجريبي

3.2 g of t-butyl [2-(3-bromopyridine-2-carboxamido)ethyl]carbamate were heated to reflux for 4 hours with 3.5 ml of methylene chloride and 3.5 ml of trifluoroacetic acid. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in ethanol and the solution was treated with an equimolar amount of ethanolic hydrochloric acid. The hydrochloride was recrystallized from methanol/ether, whereby there was obtained N-(2-aminoethyl)-3-bromopyridine-2-carboxamide hydrochloride as white crystals, m.p. 279°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04764522uspto-grants-1988_08