反応 #1069769
ord-f811ec377c934eb9b5c669d0d761692b
反応条件
温度
140°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他while collecting the methanol condensate
- 2温度The reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm)
- 3workup.DISTILLATIONto distill off excess diethanolamine
- 4workup.DISSOLUTIONThe highly viscous oily residue was dissolved in an equal volume of acetone
- 5その他The resulting crystalline solid was collected
- 6洗浄washed with acetone
- 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.