2,4-carbon-oxo-bridged pyrimidine cyclized product and its preparation method and application
A technology of base pyrimidine and cyclized compound, which is applied in the field of 2,4-carbon-oxygen bridge pyrimidine cyclized compound and its preparation, and can solve the problems that have not been reported in the literature.
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Embodiment 19
[0024] Preparation of Example 19-Methyl-2,5-dioxa-7,10-diazabicyclo[4.3.1]dec-1(10),6,8-triene
[0025] Suspend 10.0g (79mmol) of 5-methyluracil in 102g hexamethyldisilazane amine (635mmol), add 0.1g ammonium sulfate and heat to reflux, react overnight, until the reaction solution is clear, evaporate under reduced pressure to recover excess Hexamethyldisilazane; add 80mL of dried 1,2-dichloroethane to the residue, dissolve and cool to 5°C, slowly add 7g of SnCl 4 and 10mL of 1,2-dichloroethane, after dropping, the reaction solution was heated to a slight reflux state until the completion of the reaction was detected by TLC. Cool the reaction solution to 5-10°C, add saturated NaHCO under stirring 3 Aqueous solution, to neutral, precipitated, precipitated as Sn hydroxide, filtered, concentrated the filtrate under reduced pressure, removed the reaction solvent and half the volume of water, cooled and stood still, precipitated the product solid, filtered, and then purified by wat...
Embodiment 2
[0035] On the basis of embodiment 1, apply above-mentioned catalyst SnCl 4 , raw material ratio, reaction conditions and operation methods, change the substituent on the uracil ring and 1, n-dihaloalkane (n=0,1,2), the resulting 2,4-carbon-oxygen bridging pyrimidine ring The yields of the compounds are shown in Table 1 below.
[0036] Table 1 The yield of 2,4-carbon-oxo-bridged pyrimidine cyclizations corresponding to different substituents
[0037]
[0038]
Embodiment 3
[0040] On the basis of Example 1, apply the above-mentioned raw material ratio, reaction conditions and operation method, change catalyst ZnCl 2 , substituents on the uracil ring and 1, n-dihaloalkane (n=0,1,2), the yield of the obtained 2,4-carbon-oxygen bridging pyrimidine cyclization is shown in Table 2.
[0041] Table 2 The yields of 2,4-carbon-oxygen-bridged pyrimidine cyclizations corresponding to different substituents and catalysts
[0042]
[0043]
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