在催化剂过氧磷钨酸十二烷基吡啶盐(Cat-PW4)的作用下,α-蒎烯与H2O2反应生成主要产物(3R,4R)-4,7,7-三甲基-6-氧杂二环[3.2.1]辛烷-3,4-二醇。不同反应条件对反应转化率和选择性的实验结果表明,最佳反应条件为:12.8 mmolα-蒎烯、5 m ...在催化剂过氧磷钨酸十二烷基吡啶盐(Cat-PW4)的作用下,α-蒎烯与H2O2反应生成主要产物(3R,4R)-4,7,7-三甲基-6-氧杂二环[3.2.1]辛烷-3,4-二醇。不同反应条件对反应转化率和选择性的实验结果表明,最佳反应条件为:12.8 mmolα-蒎烯、5 m L溶剂三氯甲烷、0.2 g催化剂、3.3 m L 30%H2O2,反应温度40℃,反应时间3 h,α-蒎烯转化率和产物的选择性分别为94.7%和39.8%。反应结束后,该产物存在于水相和有机相中,通过萃取和重结晶分离提纯,得率11%,纯度达到98%;其分子结构通过红外光谱、紫外光谱、1H核磁共振谱、13C核磁共振谱、低分辨率质谱及高分辨率质谱确证。展开更多
In order to obtain the key intermediate of vandetanib,4-chloro-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline was synthesized from methyl 4-[1-(tert-butoxycarbonyl) piperidin-4-ylmethoxy]-3-methoxybenzoate by ...In order to obtain the key intermediate of vandetanib,4-chloro-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline was synthesized from methyl 4-[1-(tert-butoxycarbonyl) piperidin-4-ylmethoxy]-3-methoxybenzoate by deprotection,methylation,nitration,reduction,ring formation and substitution reaction in an overall yield of 58%.The structures of the compound and its intermediates were determined by 1H NMR and MS.展开更多
文摘在催化剂过氧磷钨酸十二烷基吡啶盐(Cat-PW4)的作用下,α-蒎烯与H2O2反应生成主要产物(3R,4R)-4,7,7-三甲基-6-氧杂二环[3.2.1]辛烷-3,4-二醇。不同反应条件对反应转化率和选择性的实验结果表明,最佳反应条件为:12.8 mmolα-蒎烯、5 m L溶剂三氯甲烷、0.2 g催化剂、3.3 m L 30%H2O2,反应温度40℃,反应时间3 h,α-蒎烯转化率和产物的选择性分别为94.7%和39.8%。反应结束后,该产物存在于水相和有机相中,通过萃取和重结晶分离提纯,得率11%,纯度达到98%;其分子结构通过红外光谱、紫外光谱、1H核磁共振谱、13C核磁共振谱、低分辨率质谱及高分辨率质谱确证。
文摘In order to obtain the key intermediate of vandetanib,4-chloro-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline was synthesized from methyl 4-[1-(tert-butoxycarbonyl) piperidin-4-ylmethoxy]-3-methoxybenzoate by deprotection,methylation,nitration,reduction,ring formation and substitution reaction in an overall yield of 58%.The structures of the compound and its intermediates were determined by 1H NMR and MS.
