Preparation method of (R)-9-[2-(phosphoryl phenol methoxy)propyl]adenine
The technology of phosphorylphenol methoxy and phosphoryl methoxy is applied in the field of preparation of -9-[2-propyl]adenine, and can solve the problems of being unsuitable for industrial production, difficult to recycle, troublesome to handle, and the like, Achieve significant creativity and practical application value, improve yield, and simplify operation.
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[0062] Example one
[0063] (R)-9-[2-(phosphoryl phenol methoxy) propyl] adenine preparation method one
[0064] The compound (R)-9-[2-(phosphorylmethoxy)propyl]adenine (100.01g, 0.35mol, 1.0eq, Zhejiang Supor Pharmaceutical Co., Ltd.) represented by formula (I) was used at room temperature in 1400ml Pyridine (Shanghai Titan Chemical Co., Ltd.) was dissolved, stirred and turned into a milky solution. Triphenyl phosphite (324.04g, 1.05mol, 3.0eq, Xilong Chemical) was added to the reaction solution at room temperature and heated to reflux React at 115°C for 8 hours, the solution becomes clear first, and then a large amount of white solid precipitates, cool to about -5°C~5°C, add 1400ml acetone (Hangzhou Jiachen Chemical Co., Ltd.), stir for 1.5 hours, filter, filter cake with 100ml Wash with acetone (Hangzhou Jiachen Chemical Co., Ltd.), and dry the filter residue (white solid) at 60°C~70°C for 5 hours. The white solid obtained is the target product obtained. A total of 112.26 g of ...
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[0083] Example two
[0084] (R)-9-[2-(phosphoryl phenol methoxy) propyl] adenine preparation method 6
[0085] The compound (R)-9-[2-(phosphorylmethoxy)propyl]adenine (50.01g, 0.17mol, 1.0eq, Zhejiang Supor Pharmaceutical Co., Ltd.) represented by formula (I) was used at room temperature in 800ml Pyridine (Shanghai Titan Chemical Co., Ltd.) was dissolved, stirred and turned into a milky solution. Triphenyl phosphite (162.05g, 0.52mol, 3.0eq, Xilong Chemical) was added to the reaction solution at room temperature and heated to reflux React at 95℃ for 16 hours, the solution becomes clear first, and a large amount of white solid precipitates. Cool to about -5℃~5℃, add 800ml acetone (Hangzhou Jiachen Chemical Co., Ltd.), stir for 1.5 hours, filter, filter cake with 100ml acetone (Hangzhou Jiachen Chemical Co., Ltd.) Wash and dry the filter residue (white solid) at 60℃~70℃ for 5 hours. The obtained white solid is the target product obtained. A total of 52.77 g of white solid is obtaine...
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[0087] Example three
[0088] (R)-9-[2-(phosphoryl phenol methoxy) propyl] adenine preparation method seven
[0089] The compound (R)-9-[2-(phosphorylmethoxy)propyl]adenine (100.00g, 0.35mol, 1.0eq, Zhejiang Supor Pharmaceutical Co., Ltd.) represented by formula (I) was used at room temperature in 1400ml Pyridine (Shanghai Titan Chemical Co., Ltd.) was dissolved, stirred and turned into a milky solution. Triphenyl phosphite (1081.15g, 3.48mol, 10.0eq, Xilong Chemical) was added to the reaction solution at room temperature and heated to reflux React at 100℃ for 12 hours, the solution will become clear first, and then a large amount of white solid will precipitate. Cool to about -5℃~5℃, add 1400ml acetone (Hangzhou Jiachen Chemical Co., Ltd.), stir for 1.5 hours, filter, filter cake Wash with 100ml of acetone (Hangzhou Jiachen Chemical Co., Ltd.), and dry the filter residue (white solid) at 60°C~70°C for 5 hours. The obtained white solid is the target product. A total of 113.71 g of...
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