تفاعل #1069769
ord-f811ec377c934eb9b5c669d0d761692b
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
140°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىwhile collecting the methanol condensate
- 2درجة الحرارةThe 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
- 5أخرىThe resulting crystalline solid was collected
- 6غسيلwashed with acetone
- 7أخرىdried
الإجراء التجريبي
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.