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化学学报
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化学学报 ›› 1963, Vol. 29 ›› Issue (1): 54-57. 上一篇    下一篇

研究简报

甲氧基的快速微量测定法

吳京香   

  1. 中国科学院药物研究所
  • 投稿日期:1962-01-31 发布日期:2013-06-03

A RAPID METHOD FOR THE MICRODETERMINATION OF METHOXYL GROUP

WU JING-XIANG   

  1. Institute of Materia Medica, Academia Sinica
  • Received:1962-01-31 Published:2013-06-03

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目前应用的甲氧基微量测定法,一般均依据zeisel法[1]的原理。我们数年来用Pregl的微量法[2]作分析,但感到该法有如下缺点:1.分析速度仍不够快。一般样品的分析,仅蒸馏就要一小时。含数甲氧基的样品的分析时间还要长。例如盐酸罂粟碱含有四个甲氧基,蒸馏时间就要一小时半左右。如缩短蒸馏时间,则需加快通气速度或提高分解温度,但这往往使甲氧基的分解反应或所产生的碘甲烷与溴的反应不完全。

A modified apparatus as well as a procedure for the determination of methoxyl group was described.The main features were as follows: A reservoir with a siphon tube (B1) or a cock (Bz) was used,and the reaction solution was heated vigorously and made to circulate quickly so that the time required for the determination could be shortened.For instance,by Pregl's method the reaction of papaverine hydrochloride required 90 minutes,while by this procedure it required only 15 minutes.Usually it takes only 10 minutes for one determination.The results obrained were satisfactory.