反応 #64071

ord-1c896af0227b495fb2c8ee6f51728118

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONInto a beaker, are added
  2. 2
    workup.STIRRINGThe reaction medium is stirred
  3. 3
    温度cooled to between 5° and 10° C
  4. 4
    workup.STIRRINGThe mixture is stirred for 30 min at room temperature
  5. 5
    ろ過the clear mixture is filtered
  6. 6
    その他The filtrate is evaporated to dryness
  7. 7
    その他An oil is obtained which
  8. 8
    その他crystallizes at room temperature
  9. 9
    ろ過It is filtered on sintered glass
  10. 10
    その他The white powder obtained
  11. 11
    乾燥is dried under vacuum over phosphoric anhydride

実験手順

Into a beaker, are added, with stirring, 11.4 g (0.06 mole) of triisopropanolamine in 100 ml of isopropanol. The reaction medium is stirred and cooled to between 5° and 10° C. 19.2 g (0.06 mole) of 5-n-dodecanoylsalicylic acid are then added. The mixture is stirred for 30 min at room temperature and then the clear mixture is filtered. The filtrate is evaporated to dryness. An oil is obtained which crystallizes at room temperature. It is filtered on sintered glass. The white powder obtained is dried under vacuum over phosphoric anhydride. 29.1 g of product are obtained, equivalent to a yield of 95%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05411742uspto-grants-1995_05