反応 #1069769

ord-f811ec377c934eb9b5c669d0d761692b

試薬

なし

反応条件

温度
140°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他while collecting the methanol condensate
  2. 2
    温度The reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm)
  3. 3
    workup.DISTILLATIONto distill off excess diethanolamine
  4. 4
    workup.DISSOLUTIONThe highly viscous oily residue was dissolved in an equal volume of acetone
  5. 5
    その他The resulting crystalline solid was collected
  6. 6
    洗浄washed with acetone
  7. 7
    その他dried

実験手順

A mixture of 57.58 g (0.25 mol) dimethyl sebacate and 157.71 g (1.50 mol) of diethanolamine was heated in a 140° C. bath under nitrogen for 2.5 hrs while collecting the methanol condensate. The reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm) to distill off excess diethanolamine. The highly viscous oily residue was dissolved in an equal volume of acetone and stirred overnight. The resulting crystalline solid was collected, washed with acetone, and dried. The yield of product was 35.0 g (9.3% of theory); mp=87-98° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06861192B2uspto-grants-2005_03