山东科学
山東科學
산동과학
SHANDONG SCIENCE
2011年
5期
1-4
,共4页
冯润良%陈修毅%宋智梅%岳冬玲
馮潤良%陳脩毅%宋智梅%嶽鼕玲
풍윤량%진수의%송지매%악동령
4-二甲胺基丁醛二乙基缩醛%合成%舒马曲坦
4-二甲胺基丁醛二乙基縮醛%閤成%舒馬麯坦
4-이갑알기정철이을기축철%합성%서마곡탄
4-dimethylaminobutyraldehyde diethyl acetal%synthesis%Sumartriptan
4-二甲胺基丁醛二乙基缩醛是制备治疗偏头痛的曲坦类药物的关键中间体，其合成工艺的优劣对药物的合成成本有重要影响。本文以1-溴3-氯丙烷为起始原料，与二甲胺水溶液经相转移催化剂聚乙二醇催化得到3-二甲胺基-1-氯丙烷，然后于2-甲基四氢呋喃中与镁反应制得格氏试剂，而后与原甲酸三乙酯反应得到目标化合物。该路线总收率70．11％，路线简单、污染低、易操作、收率高。
4-二甲胺基丁醛二乙基縮醛是製備治療偏頭痛的麯坦類藥物的關鍵中間體，其閤成工藝的優劣對藥物的閤成成本有重要影響。本文以1-溴3-氯丙烷為起始原料，與二甲胺水溶液經相轉移催化劑聚乙二醇催化得到3-二甲胺基-1-氯丙烷，然後于2-甲基四氫呋喃中與鎂反應製得格氏試劑，而後與原甲痠三乙酯反應得到目標化閤物。該路線總收率70．11％，路線簡單、汙染低、易操作、收率高。
4-이갑알기정철이을기축철시제비치료편두통적곡탄류약물적관건중간체，기합성공예적우렬대약물적합성성본유중요영향。본문이1-추3-록병완위기시원료，여이갑알수용액경상전이최화제취을이순최화득도3-이갑알기-1-록병완，연후우2-갑기사경부남중여미반응제득격씨시제，이후여원갑산삼을지반응득도목표화합물。해로선총수솔70．11％，로선간단、오염저、역조작、수솔고。
4-Dimethylaminobutyraldehyde diethyl acetal is a key intermediate for the preparation of anti-migraine drugs. Its synthesis technique significantly affects the production cost of anti-migraine drugs. We catalyzed the reaction of 1-bromo-3-chloro propane and dimethylamine solution with PEG as a phase transfer catalyst, and obtained 3-dimethylamino-1-chloro propane. 3-dimethylamino-1-chloro propane reacted with magnesium and Grinard reagent was acquired. We eventually obtained our target compound by the reaction of Grinard reagent and triethyl orthoformate. The total recovery rate of our target compound was 70. 11%. The advantages of this method are simple operation, low environment pollution, high recovery rate and easy implementation.
