摘要
用薄层色谱法监测了用二氯乙酰氯、醇胺和酮合成的除草剂的安全剂N 二氯乙酰基 口恶唑烷的反应过程。方法操作简便、快速、准确。
A thin layer chromatographic procedure has been developed for the monitoring and identification of the synthesis of N dichloroacetyloxazolidine by dichloroacetyl chloride,an alcoholamine and a ketone The determination of reaction was made on the plates at room temperature The reaction liquid was spotted on the silica gel G thin layer plate and developed using solvent system,dichloromethane methanol(10∶1,V/V),until the solvent front migrated 10 cm from the starting spot Then,the separated spots(raw materials and product) were scanned in iodine About 1 hour,the raw material spots disappeared gradually and the product spots became clear,then the reaction had basically completed Compounds A,B,C and D had R\-f values of 0 71,0 76,0 75 and 0 79 respectively The repeatability of R\-f value was good The TLC procedure has also been developed for the identification of the recrystallization of crude product After recrystallization, there was one spot on the plate Then,the products were confirmed by IR,\+1HNMR and elemental analysis The separation conditions were easily obtained This method is simple,rapid,sensitive and reproducible
出处
《色谱》
CAS
CSCD
北大核心
2000年第4期374-375,共2页
Chinese Journal of Chromatography
基金
黑龙江省科委"九五"攻关课题资助!项目 (G96A1 4 1 2 )
