반응식
[C:1]([Cl:10])(=[O:9])[CH2:2][CH2:3][CH2:4][CH2:5][C:6](Cl)=[O:7].[OH:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([O:29][CH:30]([O:32][C:33](=[O:50])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][OH:49])[CH3:31])=[O:28]>C(Cl)(Cl)Cl>[Cl:10][C:1]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([O:29][CH:30]([O:32][C:33](=[O:50])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][O:49][C:6](=[O:7])[CH2:5][CH2:4][CH2:3][CH2:2][C:1]([Cl:10])=[O:9])[CH3:31])=[O:28])=[O:7])=[O:9]참가 물질
반응 조건
- 온도
- 50 °C
실험 절차
In a three-necked round bottomed flask equipped with a reflux condenser, a glass gas inlet tube and a pressure equalizing dropping funnel was placed freshly distilled adipoyl chloride (2.60 ml, 17.50 mmol) dissolved in absolute chloroform (15 ml). The temperature was raised to ca. 50° C. and under a gentle stream of nitrogen through the solution, a solution of ethylidene bis(16-hydroxyhexadecanoate) (1.0 g, 1.75 mmol) in absolute chloroform (30 ml) was added dropwise and left at this temperature a further 3 hours after addition. The mixture was then cooled to room temperature and quickly transferred into a 50 ml round bottomed flask equipped for distillation under reduced pressure. Chloroform was first distilled off at normal pressure, then oil-pump vacuum was established and excess adipoyl chloride distilled off at ca. 75° C., 5 mbar pressure, leaving the residual title compound (1.56 g).
후처리
- customIn a three-necked round bottomed flask equipped with a reflux condenser, a glass gas inlet tube
- additionafter addition
- temperatureThe mixture was then cooled to room temperature
- customquickly transferred into a 50 ml round bottomed flask
- customequipped for distillation under reduced pressure
- distillationChloroform was first distilled off at normal pressure
- distillationexcess adipoyl chloride distilled off at ca. 75° C.
출처 및 근거
- ORD 기록
- ord-84e4216bd6154ab99c7de21ee1d2cd67
- 출처 데이터셋
- uspto-grants-1999_07
- 특허 번호
- US05919434
연결된 노트
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