反应 #6191

ord-78df409f57be4493824f38128845a8fb

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooling
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
  3. 3
    洗涤The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water
  4. 4
    其他dried
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    其他The residue was purified by column chromatography (eluent: ethyl acetate)
  7. 7
    其他to obtain the powder which
  8. 8
    洗涤was washed with hexane
  9. 9
    其他dried

实验过程

To a solution of 1.21 g (5.00 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.79 ml (20.0 mmol) of triethylamine in 50 ml of methylene chloride was added 1.65 ml (6.00 mmol) of palmitoyl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain the powder which was washed with hexane and dried to obtain 1.50 g of the desired compound (73.8%, colorless powder), mp: 84.0°-85.0° C.

来源

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