摘要
对三甲酰基甲烷(4)的合成工艺进行了改进。以溴乙酸为原料,在POCl3作用下与DMF反应得中间体2-(N,N-二甲胺基亚甲基)-1,3-双二甲基氮叶利德二盐酸盐(1);1经三水合高氯酸锂沉淀后,用MeONa/MeOH解离,18%盐酸酸化合成了4,总收率60.85%,纯度97%,其结构经1H NMR和13C NMR确证。
The synthetic process of triformylmethane（4） was improved. 4 in total yield of 60.85% with 97% purity was synthesized by the reaction of bromoacetic acid with dimethylformamide in the presence of POC13 intermediate（I）, then 1 was precipitated with lithum perchlorate trihydrate, trea- ted with MeONa/MeOH and 18% hydrochloric acid. The structure was confirmed by 1H NMR and 13C NMR.
出处
《合成化学》
CAS
CSCD
北大核心
2013年第6期757-759,共3页
Chinese Journal of Synthetic Chemistry
基金
四川省科技厅科技项目(2009GZ0167
2012FZ0129)
关键词
三甲酰基甲烷
合成
工艺改进
triformylmethane
synthesis
process improvement
