首页> 外国专利> Procedure for the obtaining of carbetoxy - siringoilmetil, reserpato (Machine-translation by Google Translate, not legally binding)

Procedure for the obtaining of carbetoxy - siringoilmetil, reserpato (Machine-translation by Google Translate, not legally binding)

机译:获得甲氧基甲酸酯的程序-siringoilmetil,reserpato(由Google翻译进行机器翻译,不具有法律约束力)

摘要

Process for obtaining the carbethoxy-siringoyl-methyl-reserpate, characterized in that 100 ml. Of anhydrous pyridine contained in a balloon and two necks are added 12 g of methyl ester and of resºrpico acid. The balloon is immersed in a cooling bath of -40º c. For about 15 minutes, after which syringoyl chloride (10 g), which is dissolved after a short time, is quickly added. The bath temperature is allowed to rise to 0º and then the reaction mass is allowed to stand at about 15ºC for about 12 hours. The solution obtained is poured into 1000 ml of hexane: a substance is filtered off and washed with small amounts of hexane. The product obtained is dissolved in methylene chloride and the solution is washed first with water and then with dilute sodium hydrate solution and finally with water again. The dehydrated solution is concentrated and chromatographed on florisil, using methylene chloride as eluent. The eluation product provides, by distillation of the solvent, a straw-white product. By crystallization from a mixture of acetone-hexane, 14 g of carbethoxy-siringoyl-methyl-reserpate are obtained. (Machine-translation by Google Translate, not legally binding)
机译:获得咔唑基-甲硅烷基-甲基-对苯二甲酸酯的方法,其特征在于100毫升。在气球和两个颈中包含的无水吡啶中加入了12克的甲基酯和Resrpico酸。将气球浸入-40ºc的冷却浴中。持续约15分钟,然后快速添加短时间后溶解的丁香酰氯(10g)。使浴温升至0℃,然后使反应物料在约15℃下静置约12小时。将获得的溶液倒入1000 ml己烷中:滤出物质并用少量己烷洗涤。将获得的产物溶解在二氯甲烷中,并将溶液首先用水洗涤,然后用稀水合硫酸钠溶液洗涤,最后再用水洗涤。浓缩脱水溶液,并在二氯甲烷上进行色谱分离,使用二氯甲烷作为洗脱剂。洗脱产物通过溶剂的蒸馏提供稻草白色产物。通过从丙酮-己烷的混合物中结晶,获得14g的甲乙氧基-甲硅烷基-甲基-对苯二甲酸酯。 (通过Google翻译进行机器翻译,没有法律约束力)

著录项

  • 公开/公告号ES257914A1

    专利类型

  • 公开/公告日1961-03-16

    原文格式PDF

  • 申请/专利权人 L. ZAMBELETTI SOCIETR PER AZIONI;

    申请/专利号ES19600257914

  • 发明设计人

    申请日1960-05-07

  • 分类号1C07CA;

  • 国家 ES

  • 入库时间 2022-08-23 18:49:58

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