6-benayl aminopurine synthetic method
A technology of benzylaminopurine and a synthetic method, applied in directions such as organic chemistry, can solve the problems of serious environmental pollution, many side reactions, phosphorus oxychloride cannot be recycled through distillation, etc., and achieves the effect of cleaning and environmental protection in the process.
Inactive Publication Date: 2018-07-17
ZHEJIANG UNIV OF TECH
View PDF5 Cites 3 Cited by
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
The main problem of existing technology is: the first step reaction, uses greatly excess phosphorus oxychloride (both as chlorination reagent and also as solvent), and side reaction is many, and productive rate is low, and excessive phosphorus oxychloride can not be obtained by distillation. Recycling can only be decomposed with water, and a large amount of phosphorus-containing wastewater is discharged. N,N-dimethylaniline needs to be recycled, and the discharged wastewater also contains N,N-dimethylaniline, which seriously pollutes the environment; the second step Reaction, in order to improve the reaction conversion rate and reaction speed, it is necessary to use an excessive amount of benzylamine, resulting in complicated separation and purification process
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View moreExamples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0021] To 5 g of hypoxanthine, add 20 mL of SOCl 2 , 0.25g DMAP, 10g BTC dissolved in 20mL SOCl 2 . Heat and add BTC / SOCl dropwise 2 . Reflux (refrigerant cooling) to complete dissolution, distill off SOCl 2 (Contains phosgene, recovered and used mechanically), evaporated (drained), cooled to room temperature, and obtained milky yellow solid (6-chloropurine and DMAP hydrochloride). Add 4g of benzylamine and 25g of triethylamine directly therein, heat to 70-80°C, or microwave heating, until the reaction of 6-chloropurine is complete (monitored by TLC), add ethanol, wash the filtered solid with ethanol, and dry to obtain 7 g of the product 6-benzylaminopurine with a brown color.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More PUM
Login to View More Abstract
The invention discloses a 6-benayl aminopurine synthetic method. The method takes hypoxanthine as a raw material, thionyl chloride is taken as a solvent, phosgene or diphosgene or triphosgene is takenas a chloride agent, 4-dimethylaminopyridine or dialkyl aminopyridine is taken as a catalyst for a reaction, after the reaction is completed, 6-chloropurine is obtained, distilled thionyl chloride and phosgene dissolved in thionyl chloride are completely used for a next reaction, and then the obtained 6-chloropurine and benzylamine are subjected to the reaction to synthesize 6-benayl aminopurineunder existence of triethylamine. During a reaction process, the used chloride agent solid triphosgene is completely decomposed to the phosgene dissolved in the solvent under existence of the catalyst4-dimethylaminopyridine, and no solid constituent is residual.
Description
technical field [0001] The invention relates to the technical field of chemical synthesis of 6-benzylaminopurine. technical background [0002] The existing synthesis process is: hypoxanthine is used as a raw material, reacted with phosphorus oxychloride in the presence of N,N-dimethylaniline to obtain 6-chloropurine, and 6-chloropurine is then reacted with benzylamine in the presence of triethylamine The following reaction is carried out to synthesize 6-benzylaminopurine. The main problem of existing technology is: the first step reaction, uses greatly excess phosphorus oxychloride (both as chlorination reagent and also as solvent), and side reaction is many, and productive rate is low, and excessive phosphorus oxychloride can not be obtained by distillation. Recycling can only be decomposed with water, and a large amount of phosphorus-containing wastewater is discharged. N,N-dimethylaniline needs to be recycled, and the discharged wastewater also contains N,N-dimethylanil...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More Application Information
Patent Timeline
Login to View More IPC IPC(8): C07D473/34
CPCC07D473/34
Inventor 李景华潘伟姣毛煜鑫章中平
Owner ZHEJIANG UNIV OF TECH
PatSnap Eureka turns technology decisions into work you can execute. Powered by our Innovation Knowledge Graph, it runs expert workflows across engineering, life sciences, materials and intellectual property. Get your review-ready output in minutes.
