合成化学
閤成化學
합성화학
CHINESE JOURNAL OF SYNTHETIC CHEMISTRY
2010年
2期
248-250,253
,共4页
6-硝基喹哪啶%Skraup-Doebner-Von Miller反应%工艺改进%合成
6-硝基喹哪啶%Skraup-Doebner-Von Miller反應%工藝改進%閤成
6-초기규나정%Skraup-Doebner-Von Miller반응%공예개진%합성
6-nitrylquinaldine%Skraup-Doebner-Von Miller Reaction%process improvement%synthesis
以I_2/KI为氧化剂,甲苯为乳化剂,对硝基苯胺(2)和巴豆醛(3)经环合反应合成了6-硝基喹哪啶(1).最佳反应条件为: 2 8.92 mmol, 甲苯10 mL, 混酸45.5 mL[V(AcOH) ∶ V(HCl)＝1 ∶ 90], n(2) ∶ n(I_2/KI)＝1 ∶ 1,于100 ℃反应4 h,收率达93.1%. 1的结构经~1H NMR, IR和元素分析表征.
以I_2/KI為氧化劑,甲苯為乳化劑,對硝基苯胺(2)和巴豆醛(3)經環閤反應閤成瞭6-硝基喹哪啶(1).最佳反應條件為: 2 8.92 mmol, 甲苯10 mL, 混痠45.5 mL[V(AcOH) ∶ V(HCl)＝1 ∶ 90], n(2) ∶ n(I_2/KI)＝1 ∶ 1,于100 ℃反應4 h,收率達93.1%. 1的結構經~1H NMR, IR和元素分析錶徵.
이I_2/KI위양화제,갑분위유화제,대초기분알(2)화파두철(3)경배합반응합성료6-초기규나정(1).최가반응조건위: 2 8.92 mmol, 갑분10 mL, 혼산45.5 mL[V(AcOH) ∶ V(HCl)＝1 ∶ 90], n(2) ∶ n(I_2/KI)＝1 ∶ 1,우100 ℃반응4 h,수솔체93.1%. 1적결구경~1H NMR, IR화원소분석표정.
6-Nitrylquinaldine(1) was synthesized by cyclization of p-nitroaniline(2) with crotonaldehyde(3) using I_2/KI as the oxidant and toluene as the emulsifier. The structure was characterized by ~1H NMR, IR and elemental analysis. The optimum reaction conditions at 100 ℃ for 4 h were as follows: 2 was 8.92 mmol;toluene was 10 mL;mixed acid[V(AcOH) ∶ V(HCl)＝1 ∶ 90] was 45.5 mL;n(2) ∶ n(I_2/KI)＝1 ∶ 1. The yield of 1 can reach 93.1% under the conditions.
