반응식
[CH:1]([NH2:4])([CH3:3])[CH3:2].CCCCCC.C([Li])CCC.[CH:16]([C:18]1[CH:23]=[CH:22][C:21]([CH:24]=[CH2:25])=[CH:20][CH:19]=1)=[CH2:17]>CCCCCC>[CH:1]([NH:4][CH2:25][CH2:24][C:21]1[CH:22]=[CH:23][C:18]([CH:16]=[CH2:17])=[CH:19][CH:20]=1)([CH3:3])[CH3:2]참가 물질
실험 절차
In a 300 ml four necked flask equipped with a thermometer, a reflux condenser, an inlet for nitrogen and a stirrer were charged 1860 ml of dry n-hexane and 148 g of iso-propylamine. While stirring the mixture, 119 ml of a 15% n-butyllithium n-hexane solution were added dropwise thereto. During the addition, the temperature was maintained at 5° C. to 7° C. The color of the solution was changed from colorless to pale yellow. After 10 minutes, 325 g of p-divinylbenzene having a purity of 96% were added to the mixture, whereby the color of the reaction mixture was changed to brown. Then, the inner temperature was elevated to 45° C., at which the reaction was continued for 6 hours. After the reaction, the reaction was terminated with ethanol and the solvent was evaporated. The residue was poured into 2 l of n-hexane and the insoluble are filtered off, followed by evaporation and distillation, whereby there were obtained 230 g of the product having a boiling point of 62° C.-64° C./0.08 mmHg.
후처리
- additionwere added dropwise
- additionDuring the addition
- temperaturethe temperature was maintained at 5° C. to 7° C
- customwas elevated to 45° C., at which
- waitwas continued for 6 hours
- customAfter the reaction
- customthe reaction was terminated with ethanol
- customthe solvent was evaporated
- additionThe residue was poured into 2 l of n-hexane
- filtrationthe insoluble are filtered off
- customfollowed by evaporation and distillation
출처 및 근거
- ORD 기록
- ord-f9a5bc7a1a1643b194ed7fc5edc01fce
- 출처 데이터셋
- uspto-grants-1982_01
- 특허 번호
- US04311799
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