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目的 由间甲氧基苯乙酮 (Ⅴ )合成 1-甲基-3-乙基-3-(3-羟基苯基)-六氢-1H-氮杂盐酸盐 (Ⅰ )。方法以间甲氧基苯乙酮 (Ⅴ )为起始原料经Willgerodt重排和氯置换成酰氯 ,然后与 4 甲氨基丁酸甲酯盐酸盐 (Ⅳ )缩合成酰胺 ,碱性环合后再乙基化 ,通过Wolff Kishner Huang和锂铝氢二步还原 ,最后成盐共八步反应得到 1-甲基-3-乙基-3-(3-羟基苯基)-六氢-1H-氮杂盐酸盐 (Ⅰ )。结果 采用价廉易得的原料、试剂和普通的反应条件、经八步反应高质量地合成了 1-甲基-3-乙基-3-(3-羟基苯基)-六氢-1H-氮杂盐酸盐 (Ⅰ )。结论 该合成法操作简便、成本低廉 ,具有工业生产价值。
Aim To synthesize 1-methyl-3-ethyl-3- (3-hydroxyphenyl) -hexahydro-1H-azepine hydrochloride from m-methoxyacetophenone (V). Methods Starting from m-methoxyacetophenone (V), Willgerodt rearrangement and chloro-substitution were carried out to form acid chlorides, and then to 4-methylaminobutyrate methyl ester hydrochloride (IV) Reethylation, two-step reduction by Wolff Kishner Huang and lithium aluminum hydride, and finally salt formation in a total of eight steps yielded 1-methyl-3-ethyl-3- (3- hydroxyphenyl) Azepine hydrochloride (I). Results The synthesized 1-methyl-3-ethyl-3- (3-hydroxyphenyl) -hexahydro- Azepine hydrochloride (I). Conclusion The synthesis method is simple, low cost, with industrial production value.