反应 #1973962

ord-70d5024c6fa54b849460b2a52395ed07

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度This mixture was heated
  2. 2
    温度to reflux
  3. 3
    workup.ADDITIONadded every 3 h
  4. 4
    温度The mixture was then refluxed for 24 h
  5. 5
    温度The mixture was then cooled
  6. 6
    浓缩concentrated under vacuum to dryness

实验过程

The product from Example 5, Part C (16.44 g, 69.3 mmol) was dissolved in toluene (200 mL). This mixture was heated to reflux and acrylic acid added over time (1 mL of acrylic acid added every 3 h, 5.23 mL total, 76.2 mmol). The mixture was then refluxed for 24 h. The mixture was then cooled and concentrated under vacuum to dryness to yield an oil as the crude title compound that was used directly in the next reaction.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08501238B2uspto-grants-2013_08