반응 #48353

ord-83011ce417e94bfbb3e2412d8e518bc5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction was concentrated
  2. 2
    기타partitioned between chloroform (5×50 mL) and 1N sodium hydroxide (50 mL)
  3. 3
    건조The organic phase was dried over magnesium sulfate
  4. 4
    농축concentrated

실험 절차

A mixture of 3,4-diaminopyridine (1.1 g, 10.1 mmol), 1-benzyl-4-piperidone (3.2 g, 16.9 mmol) sodium triacetoxyborohydride (4.0 g, 18.9 mmol), and acetic acid (10.7 mL) in dichloroethane (10 mL) was stirred for about 6 days at room temperature. The reaction was concentrated to near dryness, and partitioned between chloroform (5×50 mL) and 1N sodium hydroxide (50 mL). The organic phase was dried over magnesium sulfate and concentrated to give the title compound (2.8 g). MS 283 (M+1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745427B2uspto-grants-2010_06