반응 #1507731

ord-5512e3fd18b84bf191208f6bff00a7ac

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter complete addition the reaction
  2. 2
    온도was heated
  3. 3
    온도to reflux for 4 hours
  4. 4
    온도The reaction was cooled
  5. 5
    기타quenched by addition of water (2 ml) and 2N sodium hydroxide (4 ml)
  6. 6
    workup.ADDITIONThe reaction was diluted with ethyl acetate
  7. 7
    여과filtered through hyflo
  8. 8
    세척washing with ethyl acetate
  9. 9
    건조Dried over magnesium sulphate
  10. 10
    기타evaporated (1.2 g)

실험 절차

1-(3-Carboxyphenyl)-5-methylbenzimidazole (2 g, 0.079 mM) was dissolved in dry tetrahydrofuran (100 ml) and cooled to 0° C. Lithium aluminium hydride (7.9 ml, 1.0 M solution) was added dropwise over 10 minutes. After complete addition the reaction was heated to reflux for 4 hours. The reaction was cooled and quenched by addition of water (2 ml) and 2N sodium hydroxide (4 ml). The reaction was diluted with ethyl acetate and filtered through hyflo, washing with ethyl acetate. Dried over magnesium sulphate and evaporated (1.2 g). MS M+ 239.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06071909uspto-grants-2000_06