반응 #40824

ord-eb6ca69b6c7b4a888c638ddbdf043103

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe solution was stirred at 50° C. for 3 hours
  2. 2
    농축it was concentrated in vacuo
  3. 3
    기타The resulting crude solid was purified MPLC column chromatography (silica gel, 0-100% MeOH in ethyl acetate)

실험 절차

General Procedure M. To a solution of 5,6-diphenylpyridine-2-carbaldehyde (Compound 54, 95 mg, 0.37 mmol) and (3-amino-propyl)-phosphonic acid (51 mg, 0.37 mmol) in MeOH (3 ml) was added Bu4NOH (0.4 ml, 0.37 mmol, 1M in MeOH) under argon. The mixture was stirred at 50° C. for 30 min. before adding NaCNBH3 (23 mg, 0.37 mmol) to the mixture. The solution was stirred at 50° C. for 3 hours, and then it was concentrated in vacuo. The resulting crude solid was purified MPLC column chromatography (silica gel, 0-100% MeOH in ethyl acetate) to obtain the title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728014B2uspto-grants-2010_06