Alkylation with dialkylsulfate and diisopropylethylamine.
Alkylation with dialkylsulfate and diisopropylethylamine.
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用二烷基硫酸酯和二异丙基乙胺进行烷基化。
DOI：
10.1016/s0021-9673(01)90575-8
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发表时间：
1985
期刊：
影响因子：
--
通讯作者：
Giese,RW
中科院分区：
文献类型：
--
作者：
Nazareth,A;Joppich,M;Panthani,A;Fisher,D;Giese,RW
将茶碱（0.1mmol）溶解在装有Mininert阀（Pierce）的5-ml反应小瓶中的乙腈（0.5ml）中。加入二异丙基乙胺（0.24ml，2.5mmol）和硫酸二甲酯（0.88ml，5 mmol），并将混合物在室温下搅拌。20分钟后的高效液相色谱（HPLC）分析显示大于99%转化为与咖啡因共洗脱的单一产物。在反应1和2小时后观察到相同的色谱图。通过薄层色谱法（TLC）也仅观察到单一产物。为了测定产率，1小时后用等体积的水稀释反应混合物，并对等分试样进行HPLC。咖啡因被用作
Theophylline (0.1 mmol) was dissolved in acetonitrile (0.5 ml) in a 5-ml Reacti-vial fitted with a Mininert valve (Pierce). Diisopropylethylamine (0.24 ml, 2.5 mmol) and dimethylsulfate (0.88 ml, 5 mmol) were added and the mixture was stirred at room temperature. High-performance liquid chromatographic (HPLC) analysis after 20 min showed greater than 99% conversion to a single product that co-eluted with caffeine. The same chromatogram was observed after 1 and 2 h of reaction. Only a single product was also evident by thin-layer chromatography (TLC). In order to determine the yield, the reaction mixture after 1 h was diluted with an equal volume of water and aliquots were subjected to HPLC. Caffeine was used as an