反应 #5491

ord-0675e965fa4340e2acbd5041468c8136

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction is quenched
  2. 2
    温度by cooling to 0° C.
  3. 3
    workup.ADDITIONadding concentrated hydrochloric acid (20 mL)
  4. 4
    workup.ADDITIONdiluting with water
  5. 5
    萃取extracting several times with ethyl acetate
  6. 6
    干燥The combined organic layers are dried (MgSO4)
  7. 7
    其他the solvent is evaporated

实验过程

Trans 3-mercaptomethyl-2-oxo-1-azacyclodecane-10-carboxylic acid (0.75 g, 3.06 mmol) is dissolved in pyridine (20 mL). Acetyl chloride (0.26 g, 3.37 mmol) is added, and the reaction is stirred at room temperature overnight. The reaction is quenched by cooling to 0° C., adding concentrated hydrochloric acid (20 mL), diluting with water, and extracting several times with ethyl acetate. The combined organic layers are dried (MgSO4), and the solvent is evaporated to give trans 3-(acetylthiomethyl)-2-oxo-1-azacyclodecane-10-carboxylic acid, MS:M+1=288.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05244889uspto-grants-1993_09