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Intermediate 12,4-Dibromo-5-methylpyrimidineTo thymine (3.7 g, 29 mmol) and phosphorus(V) oxybromide (25.0 g, 87.2 mmol) in acetonitrile (CH3CN) (150 mL) at 0 0C was added portion wise K2CO3 (12.1 g, 87.2 mmol). The mixture was allowed to warm to room temperature and then heated to 80 0C for 3 days. The reaction mixture was poured onto ice and the pH of the resulting slurry was adjusted to pH 7 by addition of K2CO3(S). The aqueous layer was extracted with methylene chloride (CH2Cl2). The organic layer was washed with brine, dried (MgSO4), filtered and concentrated. Purification by flash chromatography on silica gel (0 - 30 % ethyl acetate (EtOAc)/hexanes) afforded the desired product (7.1 g, 96%) as a white solid. LC-MS (ES) m/z = 251 , 253 and 255 [M+H]+.
1-(2-deoxy-β-D-erythro-pentofuranosyl)-5-hydroxy-5-methylhydantoin[ No CAS ]
trans-5,6-dihydroxy-5,6-dihydrothymidine[ No CAS ]
N-(2-deoxy-β-D-erythro-pentouranosyl)([2-hydroxypropanoyl]carbamoyl)carbamic acid[ No CAS ]
[ 5116-24-5 ]
[ 41308-58-1 ]
[ 67145-02-2 ]
[ 65-71-4 ]
cis et trans 6-hydroxy-5,6-dihydrothymidine[ No CAS ]
[ 5627-00-9 ]
[ 38241-09-7 ]
[ 4494-26-2 ]
Yield
Reaction Conditions
Operation in experiment
at 25℃; for 0.5h;Sonication; Inert atmosphere;
General procedure: dT was purchased from Pharma Waldhof and used as such. All solutions were prepared in water purified by a Cascada Lab Water Systems and of resistivity 18.2 MOmega cm. Solutions of dT (10-4 mol/L, 250 mL) was subjected to sonolysis at four different frequencies (200, 350, 620 and 1000 kHz) at three different power densities, 10.5, 24.5 and 42 W/mL for 2 h. Two frequencies (620 kHz and 1 MHz), among the four studied, fall under the range used for the surgical non disruptive applications. The sonolysis was carried out in a glass reactor with an L3 ELAC Nautik ultrasound generator powered by an Allied Signal R/F generator (T & C power conversion, Model AG 1006). For the experiments under argon saturated atmosphere, the solution was bubbled with argon gas for half an hour at a pressure of 5 psi prior to sonolysis and Ar was bubbled throughout the experiment. Sonolysis was carried out only at a power density of 42 W/mL under argon atmosphere, where there was maximum degradation in the case of aerated conditions. Two transducers were used with resonances 212 and 620 kHz and 350 and 1000 kHz respectively. The temperature was maintained at 25 ± 1 C.
1-(2-deoxy-β-D-erythro-pentofuranosyl)-5-hydroxy-5-methylhydantoin[ No CAS ]
trans-5,6-dihydroxy-5,6-dihydrothymidine[ No CAS ]
5-formyl-5,6-dihydroxy-5,6-dihydro-2’-deoxyuridine[ No CAS ]
N-(2-deoxy-β-D-erythro-pentouranosyl)([2-hydroxypropanoyl]carbamoyl)carbamic acid[ No CAS ]
[ 5116-24-5 ]
[ 65-71-4 ]
[ 5627-00-9 ]
[ 38241-09-7 ]
[ 4494-26-2 ]
Yield
Reaction Conditions
Operation in experiment
With air; at 25℃; for 1h;Sonication;
General procedure: dT was purchased from Pharma Waldhof and used as such. All solutions were prepared in water purified by a Cascada Lab Water Systems and of resistivity 18.2 MOmega cm. Solutions of dT (10-4 mol/L, 250 mL) was subjected to sonolysis at four different frequencies (200, 350, 620 and 1000 kHz) at three different power densities, 10.5, 24.5 and 42 W/mL for 2 h. Two frequencies (620 kHz and 1 MHz), among the four studied, fall under the range used for the surgical non disruptive applications. The sonolysis was carried out in a glass reactor with an L3 ELAC Nautik ultrasound generator powered by an Allied Signal R/F generator (T & C power conversion, Model AG 1006). For the experiments under argon saturated atmosphere, the solution was bubbled with argon gas for half an hour at a pressure of 5 psi prior to sonolysis and Ar was bubbled throughout the experiment. Sonolysis was carried out only at a power density of 42 W/mL under argon atmosphere, where there was maximum degradation in the case of aerated conditions. Two transducers were used with resonances 212 and 620 kHz and 350 and 1000 kHz respectively. The temperature was maintained at 25 ± 1 C.
With dihydrogen peroxide; 1-hydroxy-1,2,3-benzotriazine-4(3H)-one; In water; at 130℃; for 3h;Autoclave;
Add 100 g of thymine and 300 mL of water to the autoclave, and add 35 mL of hydrogen peroxide at a concentration of 30percent.15 g of 1-hydroxy-1,2,3-benzotriazine-4(3H)-one and 35 g of the catalyst prepared in Example 3, replacing the inside of the autoclave with an oxygen atmosphere, and heating to 130 ° C for 3 h.The reaction solution was cooled, filtered, concentrated, and placed in an ice-water mixture to cool.150 g of a white solid was precipitated, the yield was 96.1percent, and the purity was 99.3percent.