The Nitrendipine synthesis process improvement
6.5 [5] , publicly chartered 87-126159 (CA1987,
ralph lauren polo, 107:19 / 819z) C6] Huang Huiqin such as : Journal of Shandong University (Natural Science rebel ) 198 . (4) 86 [7 ] PieroVetal : ArchPharm ( IVeinheim ) [ July 5 , the 983316:752 I1090 year income gather in harvest ] the Chinese pharmaceutical industry magazine ChineseJournalof ~ harmo ccuticals1991 . zz (5 ) '205 entire reaction process without the toxic and hazardous solvents , simple operation , process equipment ,
tiffany deutschland, cost reduction, and j in industrial production . Part of an experiment , amino crotonic acid methyl ester (2) of methyl acetoacetate 100ml ( 0.93mo1 ) , anhydrous ethanol 20m1 added to the reaction bottle , ice - salt bath cooling , through dry ammonia 4h , frozen overnight and filtered solids with ethanol and recrystallization a white crystalline 89g , mp82N83 ° C , the yield of 90, Chu (Ref. : mp82 83 C , the yield of 76, Chu ) , 2 - ( 3 - nitro benzyl ) acetyl ethyl acetate (3) ethyl acetoacetate 4O.5ml ( 0.32mo1 ) to ~ into the reaction flask in ice - salt bath cooling and stirring dropping concentrated sulfuric acid 3.8m1 . mixing batches to join 5min between nitrobenzene formaldehyde 24g ( o.16mot ), stirring h, frozen overnight , filtered, washed with water to pH5 - too pale yellow crystalline 32.6g, mp103N107'C, yield 78% ( literature : mp106 ° C yield 85% ) . Third, nitrendipine (I) will be added to the reaction flask, 210.1g (0.09mo1) and 323.5g (0.09mo1) heated to 75 ¨ C. The stirring Slightly reduced pressure ,
ugg boots 2012, 78 to 84 . C-reactive 4 h , overnight , filtered, ethanol recrystallization ,
Abercrombie Deutschland, have fluorescent yellow crystalline powder beam 26.7g mp158 . ~ 159 ° C , yield 80.5 Jue ( literature : mp158 ~ 159 C , yield 78% ) comply with pharmaceutical standards of Shandong Province Acknowledgements This article Cheng Liu Rufang chief engineer to review the analysis by instructions from the analysis chamber Du brick engineer .
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