反应 #6227

ord-78e604ab97a5457d90db9847ffc8eaa3

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water
  2. 2
    其他dried
  3. 3
    workup.DISTILLATIONThen the solvent was distilled off
  4. 4
    其他The residue was purified by column chromatography (eluent: ethyl acetate)

实验过程

In 250 ml of methylene chloride was dissolved 22.2 g (200 mmol) of 4-mercaptopyridine and 27.9 ml (200 mmol) of triethylamine. Thereto was added 18.1 g (200 mmol) of 3-bromo-1-propanol. The mixture was stirred at room temperature for 3 hours. The reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water and dried. Then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 21.3 g of the desired compound (yield: 62.9%, yellow oil).

来源

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