반응 #2273244

ord-cc4c9277c3824a718eece4e91adfe488

시약

없음

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 12 h
  2. 2
    기타Reaction mixture
  3. 3
    농축was concentrated in vacuo

실험 절차

A solution of 4-bromo-5-aminobenzimidazole (0.22 g, 0.97 mmol) and ISA (0.34 g, 2.5 mmol) in 5 ml of isobutanol was stirred at reflux for 12 h. Reaction mixture was concentrated in vacuo and subjected to silica gel column chromatography (NH3 saturated 20% MeOH/EtOAc) to yield 0.23 g (0.83 mmol, 84%) of the product. The product obtained was converted to the fumarate salt and recrystallized from MeOH to afford 0.12 g (30%) of the product as a white solid: mp 199-202° C.; Anal. Calc. for C10H10N5Br.1.0C4H4O4.0.7H2O requires C, 41.13; H, 3.80; N, 17.13. Found: C, 41.60; H, 3.81; N, 16.97.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06403626B1uspto-grants-2002_06