摘要
以(S)-2,6-二氨基-4,5,6,7-四氢苯并噻唑(3)为原料,经缩合、还原反应制得普拉克索(2);2与盐酸成盐后制得盐酸普拉克索一水合物(1),其结构经1H NMR,13C NMR,IR和MS(ESI)确证。研究了溶剂、反应温度、投料比γ[n(3)∶n(正丙醛)]、析晶终止温度和精制降温速度对1收率的影响。结果表明:在最佳反应条件(无水甲醇为溶剂,γ=1.0∶1.8,于-15^-20℃反应,析晶终止温度为-5^-10℃)下,最高收率可达61.5%。
Pramipexole（2） was prapared from（S）-2,6-diamino-4,5,6,7-tetrahydro-benzothiazole（3）by condensation and reduction reaction. Pramipexole hydrochloride（1） was synthesized from 2 via salification and drecrystallization. The structure was confirmed by1 H NMR,13 C NMR,IR and MS（ESI）. The effect of reaction solvent,reaction temperature,the raw ratio γ[n（3） ∶ n（n-propionaldehyde） ] and terminational temperature of crystallization and cooling speed of refining on the yield of 1were invistigated. The yield was up to 61. 5% under the optimized conditons（anhydrous methanol as reaction solvent,γ = 1. 0∶ 1. 8,reaction at-15 --20 ℃,terminational temperature of crystallization was-5 --10 ℃）.
作者
黄斌
李景
何作瑜
谢银彩
王诗红
HUANG Bin LI Jing HE Zuo-yu XIE Yin-cai WANG Shi-hong(The Fifth Affiliated（Zhuhai） Hospital, Zunyi Medical College, Zhuhai 519100, China)
出处
《合成化学》
CAS
CSCD
2017年第3期261-264,共4页
Chinese Journal of Synthetic Chemistry
基金
贵州省科学技术基金资助项目(黔科合LH字[2014]7560号)
