石油化工高等学校学报
石油化工高等學校學報
석유화공고등학교학보
JOURNAL OF PETROCHEMICAL UNIVERSITIES
2014年
6期
20-23
,共4页
宫哲%王德慧%宋官龙%赵德智
宮哲%王德慧%宋官龍%趙德智
궁철%왕덕혜%송관룡%조덕지
ω-吖啶戊酸%催化反应%路易斯酸%质子酸
ω-吖啶戊痠%催化反應%路易斯痠%質子痠
ω-아정무산%최화반응%로역사산%질자산
5-(Acridin-9-yl)pentanoic acid%Catalytic reaction%Lewis acid%Bronsted acid
在路易斯酸和质子酸既作为催化剂又作为溶剂的条件下,二苯胺与己二酸通过酸催化环合反应生成ω-吖啶戊酸。分别考察了常见催化剂、反应时间、反应温度、催化剂用量、底物投料比等因素对最终产品收率的影响。实验结果表明,HF 活性较高、反应时间6 h、反应温度60℃、n (催化剂)/n (底物)=3、n (二苯胺)/n (己二酸)=1∶3时,其产品ω-吖啶戊酸最高收率达到82.6%。通过 NMR、MS 和元素分析对产品ω-吖啶戊酸进行表征,结果表明产物为ω-吖啶戊酸。HF 作为催化剂使得反应温度低、产品易于分离精制、产品纯度较高。
在路易斯痠和質子痠既作為催化劑又作為溶劑的條件下,二苯胺與己二痠通過痠催化環閤反應生成ω-吖啶戊痠。分彆攷察瞭常見催化劑、反應時間、反應溫度、催化劑用量、底物投料比等因素對最終產品收率的影響。實驗結果錶明,HF 活性較高、反應時間6 h、反應溫度60℃、n (催化劑)/n (底物)=3、n (二苯胺)/n (己二痠)=1∶3時,其產品ω-吖啶戊痠最高收率達到82.6%。通過 NMR、MS 和元素分析對產品ω-吖啶戊痠進行錶徵,結果錶明產物為ω-吖啶戊痠。HF 作為催化劑使得反應溫度低、產品易于分離精製、產品純度較高。
재로역사산화질자산기작위최화제우작위용제적조건하,이분알여기이산통과산최화배합반응생성ω-아정무산。분별고찰료상견최화제、반응시간、반응온도、최화제용량、저물투료비등인소대최종산품수솔적영향。실험결과표명,HF 활성교고、반응시간6 h、반응온도60℃、n (최화제)/n (저물)=3、n (이분알)/n (기이산)=1∶3시,기산품ω-아정무산최고수솔체도82.6%。통과 NMR、MS 화원소분석대산품ω-아정무산진행표정,결과표명산물위ω-아정무산。HF 작위최화제사득반응온도저、산품역우분리정제、산품순도교고。
5-(acridin-9-yl)pentanoic acid was prepared using N-phenylaniline and adipic acid as raw materials by cyclization reaction.Lewis acid and Bronsted acid were chosen as catalysts under the condition of solvent-free.The effect of sort of catalysts,reaction time,reaction temperature,the amount of catalysts and the mole ratio of reactants on the yields of final products were investigated.The results showed that the yeild of 5-(acridin-9-yl)pentanoic acid can reach 82.6% under the following experimental conditions:HF with high catalytic activity,the reaction time 6 h,the reaction temperature 60 ℃,3 times molar ratio of the amount of catalyst to substrate,molar ratio of N-phenylaniline to adipic 1 ∶ 3.NMR,MS and elemental analysis were used to characterize the product of 5-(acridin-9-yl)pentanoic acid.The temperature of reaction with HF catalyst was low.The product can be easily seperated and purified with high purity.