Fischer法合成2-苄基-2,3,4,5-四氢-1H-吡啶并[4,3-b]吲哚工艺的改进  

Improved Fischer Method for Synthetic Process of 2-Benzyl-2,3,4,5-tetrahydro-1H-pyrido- Indole

作　　者：马强[1] 崔涛[1] 滕大为[1] 

机构地区：[1]青岛科技大学化工学院,山东青岛266042

出　　处：《化学与生物工程》2013年第6期48-51,共4页Chemistry & Bioengineering

摘　　要：采用Fischer法,以苯肼和1-苄基-4-哌啶酮为原料,首先合成苯腙化合物,再经过酸的催化重排、冷却、抽滤、洗涤、重结晶得2-苄基-2,3,4,5-四氢-1 H-吡啶并[4,3-b]吲哚,考察了投料方式、酸的选择、"一锅煮"技术、重结晶溶剂对收率的影响,确定适宜的工艺条件为:投料方式采用将苯肼滴加到1-苄基-4-哌啶酮和酸的混合液中,酸选择醋酸-盐酸(5∶1,摩尔比)、重结晶溶剂选择甲醇,在此条件下目标化合物收率(以苯肼计)达86%～93%,纯度达98%以上。Adopting Fischer method, with phenylhydrazine and 1-benzyl-4-piperidine ketone as raw materi- als, firstly hydrazone compound was synthesized, and then 2-benzyl-2,3,4,5-tetrahydro-lH-pyrido-l-4,3-b] in- dole was obtained through the acid-catalyzed rearrangement, cooling, suction filtrating, washing, and recrystalli- zation. The effects of feeding mode,acid selection,＂one-pot＂ technique and recrystallization solvent on the yieldwere investigated. The optimum process conditions were as follows, phenylhydrazine was dropwise added to a mixture solution of 1-benzyl-4-piperidone and acid,acid was a mixture of acetic acid and hydrochloric acid（the molar ratio was 5 ： 1） ,recrystallization solvent was methanol. Under above conditions,the yield of target com- pound was 86%-93% （phenylhydrazine dollars） and its purity was over 98%.

关 键 词：苯肼 2-苄基-2 3 4 5-四氢-1H-吡啶并[4 3-b]吲哚 重结晶 工艺改进 

分 类 号：TQ463.4[化学工程—制药化工]