反应 #6236

ord-9078b706d8484760a405cf9de643eb4b

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤insoluble materials were filtered off
  2. 2
    workup.DISTILLATIONThe volatile component in the filtrate was distilled off
  3. 3
    workup.ADDITIONchloroform was added to the residue
  4. 4
    洗涤The mixture was washed with brine
  5. 5
    干燥dried over potassium carbonate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off

实验过程

Hydrazine monohydrate [2.99 ml (61.6 mmol)] was added to a suspension of 5.80 g (20.5 mol) of 4-(3-phthalimidopropyloxy)pyridine in 50 ml of ethanol, and the mixture was stirred at room temperature for 3 hours. 100 ml of ethyl acetate was added and insoluble materials were filtered off. The volatile component in the filtrate was distilled off and then chloroform was added to the residue. The mixture was washed with brine and dried over potassium carbonate. The solvent was distilled off to obtain 2.99 g of the desired compound (yield: 99.5%, pale yellow oil).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05246948uspto-grants-1993_09