摘要
叙述了以叔丁醇、金属钠为原料,用双光气替代光气合成新型氨基保护剂二碳酸二叔丁酯的工艺研究。合成三步总收率大于88%,文献最高82%,成品含量大于99%。研究了固体光气、双光气解聚为光气的历程和工艺。并从产业化角度对反应溶剂、水分、pH值、反应压力和金属离子等影响产品得率、稳定性和品质的因素作了研究和探讨。
This article is about the process research on synthesis of di-tert-butyl dicarbonate(diboc), a certain kind of amino-group protective agent, which was prepared by using ten-butyl alcohol and metal Na as the main raw materials via diphosgene, instead of phosgene. The total yield was 88% or above, while the documented highest yield was 82%, and the purity of the final product was 99% (min.). The mechanism and technique of depolymerization from triphosgene and diphosgene to phosgene were studied. Meanwhile, from the industrialization point of view, some factors like solvent, moisture, pH value, reaction pressure and metal ions, which affect the yield, stability and purity of the final product, were also studied and discussed.
出处
《上海化工》
CAS
2006年第2期22-27,共6页
Shanghai Chemical Industry
关键词
氨基保护剂
合成
双光气
二碳酸二叔丁酯
Amino-group pyteetive agent
Synthesis
Diphosgene
Di-tert-butyl dicarbonate