反应 #2307990

ord-c5190574bfae43199d5ee8c01e2edb58

试剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After completion of the reaction the organic solvent
  2. 2
    其他was removed by evaporation
  3. 3
    workup.ADDITIONthe resulting solution was diluted by 15 ml NaHCO3 solution (saturated)
  4. 4
    萃取Then the mixture was extracted three times by 10 ml of acetic acid ethyl ester
  5. 5
    workup.ADDITIONby adding HCl (15% in water)
  6. 6
    萃取The resulting mixture was extracted three times by 30 ml of acetic acid ethyl ester
  7. 7
    其他The organic layer was separated
  8. 8
    洗涤washed three times with brine
  9. 9
    干燥dried (Na2SO4)
  10. 10
    其他evaporated

实验过程

3 (4.2 g, 9.6 mmol) was dissolved in 30 ml of water/acetone (1/5 v/v) and 11.6 ml NaOH (1N) where added. After completion of the reaction the organic solvent was removed by evaporation and the resulting solution was diluted by 15 ml NaHCO3 solution (saturated). Then the mixture was extracted three times by 10 ml of acetic acid ethyl ester. After that the solution was brought to pH2 by adding HCl (15% in water). The resulting mixture was extracted three times by 30 ml of acetic acid ethyl ester. The organic layer was separated and washed three times with brine, dried (Na2SO4) and evaporated.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07368421B2uspto-grants-2008_05