反应 #63200

ord-1cbcb9c30bbd4eff8ca4edb9d8fd9e75

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe solution was stirred for a further hour at 5° C.
  2. 2
    其他the catalyst was removed by filtration
  3. 3
    浓缩the filtrate was concentrated to dryness in vacuo

实验过程

Hydrazine hydrate (7 ml) in methanol (25 ml) was added with stirring over 25 minutes to a cooled (5°-10° C.) solution of 2-[3-(5,6,7,8-tetrahydroquinol-8-yl)propylamino-3-nitro-5-(pyrid-3-ylmethyl)pyridine (6.1 g) in methanol (300 ml) containing Raney Nickel (ca. 12 g). The solution was stirred for a further hour at 5° C., the catalyst was removed by filtration and the filtrate was concentrated to dryness in vacuo giving the title compound as an orange oil (theoretical yield assumed) which was used unpurified in the next reaction.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04764519uspto-grants-1988_08