90877-48-8Relevant articles and documents
In-situ and one-step preparation of protein film in capillary column for open tubular capillary electrochromatography enantioseparation
Li, Ling,Xue, Xuqi,Zhang, Huige,Lv, Wenjuan,Qi, Shengda,Du, Hongying,Manyande, Anne,Chen, Hongli
supporting information, p. 2139 - 2142 (2021/04/07)
In this work, the phase-transitioned BSA (PTB) film using the mild and fast fabrication process adhered to the capillary inner wall uniformly, and the fabricated PTB film-coated capillary column was applied to realize open tubular capillary electrochromatography (OT-CEC) enantioseparation. The enantioseparation ability of PTB film-coated capillary was evaluated with eight pairs of chiral analytes including drugs and neurotransmitters, all achieving good resolution and symmetrical peak shape. For three consecutive runs, the relative standard deviations (RSD) of migration time for intra-day, inter-day, and column-to-column repeatability were in the range of 0.3%–3.5%, 0.2%–4.9% and 2.1%–7.7%, respectively. Moreover, the PTB film-coated capillary column ran continuously over 300 times with high separation efficiency. Therefore, the coating method based on BSA self-assembly supramolecular film can be extended to the preparation of other proteinaceous capillary columns.
Preparation method of terbutaline
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Paragraph 0038; 0042-0043, (2020/12/05)
The invention belongs to the field of pharmacy, and particularly relates to a preparation method of terbutaline. The method comprises: S1, adding a compound I and dichloromethane into a reaction kettle, stirring and dissolving, and then adding anhydride, S2, after the reaction is finished, adding dilute alkaline water into the system, fully stirring and washing, collecting a dichloromethane phase,and carrying out reduced pressure distillation to obtain a yellow oily matter, namely a compound II, S3, adding the compound II, ethyl acetate, tert-butylamine, sodium hydroxide and an oxidation protective agent into the reaction kettle, and S4, after the reaction in the step S3 is finished, adding purified water into the system to wash the reaction solution in the step S3, collecting an ethyl acetate phase, and carrying out reduced pressure distillation on the ethyl acetate phase to obtain terbutaline. According to the technical scheme provided by the invention, the post-reaction treatment difficulty is reduced, so that an intermediate compound is easily separated from a reaction system, meanwhile, side reactions such as epoxy bond hydrolysis are avoided, and the stability and yield of the final product terbutaline are improved.
Preparation method of terbutaline sulfate
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Paragraph 0017; 0029; 0032; 0034; 0037; 0039; 0042; 0044, (2020/04/29)
The invention discloses a preparation method of terbutaline sulfate, wherein the method comprises the following steps: carrying out a bromination reaction on 3,5-dihydroxyacetophenone as a raw material by using a bromination reagent without hydroxyl protection, carrying out reduction and ring closing, carrying out a ring-opening reaction with tert-butylamine, and finally forming a salt with sulfuric acid to obtain terbutaline sulfate. According to the method, the defects of requirement of deprotection after hydroxyl protection, use of various high-risk highly toxic reagents, long reaction stepand low yield in the prior art are overcome.