公开(公告)号：KR1020080076149A

公开(公告)日：2008-08-20

申请号：KR1020070015680

申请日：2007-02-15

Applicant: 안국약품 주식회사

Inventor： 진경용 ,  문병헌 ,  정창우 ,  권오준 ,  배경호 ,  원덕권 ,  어진

IPC: C07D473/10

Abstract: A method for preparation of 3,7-dimethylxanthine is provided to reduce the costs for preparation by removing a cost-consuming deprotection process, improve the convenience and reproducibility of reaction by performing methylation in organic phase, and enhance purity and yield of 3,7-dimethylxanthine. A method for preparation of 3,7-dimethylxanthine represented by the formula(1) comprises the steps of: (a) suspending 3-methylxanthine represented by the formula(2) in solvent of sulfolane represented by the formula(3); and (b) reacting the suspension with methylating agent selected from methyl p-toluenesulfonate, methyl methanesulfonate and a mixture thereof in the presence of base selected from potassium hydroxide, sodium hydroxide and sodium hydride at pH 9-10, wherein the reaction temperature is -10 to 100°C. Further, a volume ratio of the sulfolane and water is 3:1 to 1:3.

Abstract translation: 提供了制备3,7-二甲基黄嘌呤的方法，通过去除成本低的去保护方法来降低制备成本，通过在有机相中进行甲基化提高反应的方便性和再现性，提高了纯度和产率3,7 -dimethylxanthine。 由式（1）表示的制备3,7-二甲基黄嘌呤的方法包括以下步骤：（a）将由式（2）表示的3-甲基黄嘌呤悬浮在由式（3）表示的环丁砜的溶剂中; 和（b）使该悬浮液与选自甲基对甲苯磺酸甲酯，甲磺酸甲酯及其混合物的甲基化剂在选自氢氧化钾，氢氧化钠和氢化钠的碱的存在下，pH 9-10下反应，其中反应温度为 - 10〜100℃。 此外，环丁砜和水的体积比为3:1至1:3。