反应 #78096

ord-64f1299de44543f89d5a238bdc68376c

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    温度to reflux for 1.5 hours whereafter the solvent
  3. 3
    其他was removed under reduced pressure
  4. 4
    其他The residue was triturated with a mixture of diethyl ether and ethanol

实验过程

To a solution of 5-acetyl-1-[3-(1-methyl-1,2,3,6-tetrahydropyrid-5-yl)phenyl]-benzimidazole (7) (free base from above) in ethanol was added O-ethyl hydroxylamine hydrochloride. The mixture was heated to reflux for 1.5 hours whereafter the solvent was removed under reduced pressure. The residue was triturated with a mixture of diethyl ether and ethanol leaving 5-acetyl-1-[3-(1-methyl-1,2,3,6-tetrahydropyrid-5-yl)phenyl]benzimidazole O-ethyl oxime (3f8) as hygroscopic crystals. Mp 138-143° C., m/e 374.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06710044B2uspto-grants-2004_03