反应 #430041

ord-ef69e2d14e8743fda5daeb2393372b0e

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度gradually warmed to room temperature
  2. 2
    温度The resulting white slurry was heated
  3. 3
    温度under reflux for 3 hours
  4. 4
    workup.WAITleft
  5. 5
    温度to cool for 10 minutes
  6. 6
    workup.ADDITIONpoured
  7. 7
    workup.STIRRINGstirring
  8. 8
    过滤The suspension was filtered
  9. 9
    其他the solid product dried

实验过程

A slurry of 2-aminobutyric acid (100 g, Aldrich) in absolute ethanol (300 ml) was stirred under nitrogen at 0° C. and thionyl chloride (120.79 g) was added dropwise. The reaction was stirred overnight at 0° C. and then gradually warmed to room temperature. The resulting white slurry was heated under reflux for 3 hours, left to cool for 10 minutes, then poured into chilled diethyl ether (600 ml) with hand stirring. The suspension was filtered and the solid product dried to give the desired product (150 g) as a white solid. 1H NMR consistent with proposed structure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05859240uspto-grants-1999_01