Cyclobutyl purine derivative or salt thereof
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reference example 1
[0250]
[0251]First Step
[0252]Under a nitrogen atmosphere, a 2.0 M lithium aluminum hydride / tetrahydrofuran solution (25 mL) was added dropwise under ice-cooling to a mixture of ethyl cis-3-aminocyclobutane-1-carboxylate hydrochloride (4.3 g) and tetrahydrofuran (43 mL) which was then stirred at room temperature for 1 hour. Water (4 mL), a 15% aqueous sodium hydroxide solution (4 mL), and water (12 mL) were added to the reaction solution, and the resulting solid was filtered off and washed with tetrahydrofuran. The solvent was distilled off under reduced pressure to give (cis-3-aminocyclobutyl)methanol (4.4 g) as a colorless oil.
[0253]Second Step
[0254]A mixture of (cis-3-aminocyclobutyl)methanol (8.5 g) obtained in the first step, 2-amino-4,6-dichloro-5-formamidopyrimidine (17.4 g), N,N-diisopropylethylamine (73 mL), ethanol (255 mL), and N-methyl-2-pyrrolidone (8.5 mL) was stirred with heating under reflux for 6 hours. The solvent was distilled off under reduced pressure, and the obt...
reference example 2-1
[0261]
[0262]A 5 M sodium methoxide / methanol solution (0.5 mL) was added to a mixture of (cis-3-(2-amino-6-chloro-9H-purin-9-yl)cyclobutyl)methanol hydrochloride (336 mg) and methanol (4.0 mL) which was then stirred at 50° C. for 5 hours. The solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:50 to 0:100, methanol:ethyl acetate=0:100 to 20:80) to give (cis-3-(2-amino-6-methoxy-9H-purin-9-yl)cyclobutyl)methanol (142 mg) as a white solid.
[0263]MS (ESI m / z): 250 (M+H)
[0264]RT (min): 0.54
reference example 2-2
[0265]
[0266]Cyclopropylamine (50 μL) was added to a mixture of (cis-3-(2-amino-6-chloro-9H-purin-9-yl)cyclobutyl)methanol hydrochloride (20 mg) and ethanol (0.5 mL) which was then irradiated with microwave (microwave reactor, 120° C., 1 hour, 2.45 GHz, 0 to 240 W). The reaction solution was purified by silica gel column chromatography (hexane:ethyl acetate=50:50 to 0:100, methanol:ethyl acetate=0:100 to 20:80) to give (cis-3-(2-amino-6-(cyclopropylamino)-9H-purin-9-yl)cyclobutyllmethanol (21 mg) as a white solid.
[0267]MS (ESI m / z): 275 (M+H)
[0268]RT (min): 0.55
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