反应 #1687640

ord-3ce417c3b828498bb3e3318faf6f929e

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe reaction mixture was stirred for additionally 24 h
  2. 2
    萃取extracted with ether
  3. 3
    干燥The combined ether phases were dried
  4. 4
    其他evaporated
  5. 5
    其他Purification by column chromatography (SiO2, eluent: ethyl acetate/methylene chloride (1:1))

实验过程

Sodium hydrogen sulfide monohydrate (0.74 g, 10.5 mmol) was added to a solution of 3 -(3-chloro-1,2,5-oxadiazol-4-yl) pyridine (1.27, 7.0 mmol) in DMF (30 ml) at room temperature and the reaction mixture was stirred for 1 h. Potassium carbonate (2.0 g, 14.5 mmol) and 1-bromo-3-phenylpropane (2.4 g, 12 mmol) were added and the reaction mixture was stirred for additionally 24 h. Water (50 ml) was added and extracted with ether. The combined ether phases were dried and evaporated. Purification by column chromatography (SiO2, eluent: ethyl acetate/methylene chloride (1:1)) gave the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE036375uspto-grants-1999_11