반응 #59086

ord-23b831165b594061af368ddb966482f7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Reaction
  2. 2
    농축concentrated
  3. 3
    기타Purification on silica gel, 50% acetone in hexanes

실험 절차

The mixture containing 4-(2-methoxy-4-(methylamino)-5-nitrophenoxy)pyridine-2-carboxylic acid (1 eq), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (2 eq), 3H-1,2,3-triazolo[4,5-b]pyridine-3-ol (1.5 eq), and diisopropylamine (5 eq) in tetrahydrofuran was stirred at room temperature for 1 hour. To this was then added ammonium chloride (2 eq) and the resulting mixture was stirred together for 48 hours. Reaction concentrated. Purification on silica gel, 50% acetone in hexanes to yield 4-(2-methoxy-4-(methylamino)-5-nitrophenoxy)pyridine-2-carboxamide as a bright yellow solid. HPLC=3.70 min; MS: MH+=319.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423150B2uspto-grants-2008_09