반응식
[C:1]([O:15]C)(=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([O:12]C)=O.[NH:17]([CH2:21][CH2:22][OH:23])[CH2:18][CH2:19][OH:20]>>[OH:20][CH2:19][CH2:18][N:17]([CH2:21][CH2:22][OH:23])[C:10](=[O:12])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([N:17]([CH2:21][CH2:22][OH:23])[CH2:18][CH2:19][OH:20])=[O:15]참가 물질
3
반응 조건
- 온도
- 140 °C
실험 절차
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.
후처리
- customwhile collecting the methanol condensate
- temperatureThe reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm)
- distillationto distill off excess diethanolamine
- dissolutionThe highly viscous oily residue was dissolved in an equal volume of acetone
- customThe resulting crystalline solid was collected
- washwashed with acetone
- customdried
출처 및 근거
- ORD 기록
- ord-f811ec377c934eb9b5c669d0d761692b
- 출처 데이터셋
- uspto-grants-2005_03
- 특허 번호
- US06861192B2
연결된 노트
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