3-(2-甲基-6-硝基苯基)-4,5-二氢异噁唑的合成研究

Synthesis of 3-(2-Methyl-6-nitrophenyl)-4,5-dihydroisoxazole

研究了常压下一锅法制备3-(2-甲基-6-硝基苯基)-4,5-二氢异噁唑的方法。原料2-甲基-6-硝基苯甲醛肟溶解后通入氯气进行氯化反应,氮气吹脱过量的氯气和生成的氯化氢后,通入乙烯、滴加缚酸剂进行环合反应得到产品。探索了溶剂、溶剂的量、反应温度和反应时间等因素对反应的影响,优化条件为以1,2-二氯乙烷为溶剂、溶剂量为原料的5倍、室温反应、通入乙烯反应8 h,反应转化率99.5%。优化条件下,收率为90.5%。

One-pot synthesis of 3-（2-methyl-6-nitrophenyl）-4,5-dihydroisoxazole under atmospheric pressure was studied. Chlorine was induced to the solution of 2-methyl-6-nitrobenzaldehyde oxime. After the chlorination process was completed, nitrogen was induced to blow off the excess chlorine and the generated hydrogen chloride. Then ethylene was introduced and the acid binding agent was added. The product was synthesized by 1,3-dipolar cycloaddition. The effects of solvent, reaction temperature and time on the reaction were explored. Optimal conditions were as followings： 1,2-dichloroethane as solvent, the amount of solvent as 5 times quality of the raw materials, room temperature reaction and ethylene reaction for 8 hours, the reaction conversion rate of 99.5% was obtained and the yield was up to 90.5%.