CAS: 144282-37-1; Tert-Butyl (S)-(5-Benzyl-5-Azaspiro[2.4]Heptan-7-yl)Carbamate

相似化合物

127199-45-5 127199-44-4 1638744-35-0

上下游产品

5-Benzyl-7(S)-Amino-5-Azaspiro[2,4]Heptane 144282-35-9

乙酰乙酰苄胺(aaba)置于(1S)-(+)-10-Camphorsulfonic Acid,吡啶,Sodium Tetrahydroborate,N-溴代丁二酰亚胺(Nbs),三甲基氯硅烷,三氟化硼乙醚,盐酸羟胺,四丁基溴化铵,Potassium Carbonate,Sodium Hydroxide体系中,用 四氢呋喃,二氯甲烷,水,1,2-二氯乙烷,N,N-二甲基甲酰胺,甲苯,乙腈 用作溶剂,化学反应 45.0H,反应生成(7S)-5-(苯甲基)5-氮杂螺[2.4]庚烷-7-基氨基甲酸叔丁酯
参考文献:一种5-苄基-7(S)-叔丁氧羰基氨基-5-氮杂螺 [2,4]庚烷的制备方法
标题:一种5-苄基-7(S)-叔丁氧羰基氨基-5-氮杂螺 [2,4]庚烷的制备方法
摘要:本发明公开了一种5-苄基-7(S)-叔丁氧羰基氨基-5-氮杂螺[2,4]庚烷的制备方法,以乙酰乙酸苄酰胺作为原料,与1,2-二氯乙烷反应得到3-环丙基乙酰乙酸苄酰胺,3-环丙基乙酰乙酸苄酰胺用nbs溴化得到1-溴-3-环丙基乙酰乙酸苄酰胺,经碱性条件作用下环化得到5-苄基-5-氮杂螺[2.4]庚烷-4,7-二酮,进一步与盐酸羟胺形成肟类化合物4-氧代-5-苄基-7-肟-5-氮杂螺[2.4]庚烷,用nabh4和三氟化硼乙醚还原得到5-苄基-7-氨基-5-氮杂螺[2.4]庚烷,运用拆分剂l-樟脑磺酸进行手性拆分得到5-苄基-7(S)-氨基-5-氮杂螺[2,4]庚烷,经与二碳酸二叔丁酯反应后得到5-苄基-7(S)-叔丁氧羰基氨基-5-氮杂螺[2,4]庚烷.本发明中间体羰基无需保护,原料易得,工艺路线简单,适合工业化生产.

专利信息

专利号:US-10358417-B2
优先权日:2016-05-06
标 题 :Method for preparing efficiently synthetic sitafloxacin intermediate (7S)-5-azaspiro[2.4]heptane-7-yl tert-butyl carbamate
发明人：LAI YINGJIE; YE DABING; LANG FENGRUI; LONG XIANGTIAN
权利人:CHEN STONE GUANGZHOU CO LTD
摘要:The present invention discloses a preparation method for efficient synthesis of sitafloxacin intermediate (7S)-5-azaspiro[2.4]heptane-7-yl-tert-butyl carbamate, comprising the following steps: reacting n nto obtainn n nreactingn n nto obtainn n nreactingn n nto obtainn n nand reactingn n nto obtainn n nIn the present invention, a single compound with a relatively high ee value can be obtained, the unnecessary waste of materials is avoided, the yield is significantly improved, the operation is simple, the industrial scale-up is easy, and the production cost is reduced.