تفاعل #1069769

ord-f811ec377c934eb9b5c669d0d761692b

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
140°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwhile collecting the methanol condensate
  2. 2
    درجة الحرارةThe 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
    أخرىThe resulting crystalline solid was collected
  6. 6
    غسيلwashed with acetone
  7. 7
    أخرىdried

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06861192B2uspto-grants-2005_03