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With Fe<SUP>II</SUP>EDTA; dihydrogen peroxide; chloranil In aq. phosphate buffer; acetonitrile at 37℃; for 1h;
Reactions of XBQs, H2O2, and 5mdC
General procedure: The basic system used in the study consisted of 0.1mM XBQ dissolved in acetonitrile (final acetonitrile concentration in the reaction mixture, 2%), 1.0mM H2O2, and 2.0mM 5mdC in 10mM phosphate buffer (pH 7.4) at 37°C for 1h unless otherwise stated. The phosphate buffer used for all experiments was pretreated with Chelex-100 ion-exchange resin (Bio-Rad Laboratories, Hercules, CA, USA; 5g/L) overnight to remove trace transition metals probably present in phosphate buffer as contaminants. The reaction solutions were directly injected into an HPLC/triple-quadrupole mass spectrometry (HPLC-MS/MS) system for analysis.
The intermediate 3 was prepared by mixing 780 ml of a NaOH solution having a mass fraction of 10%, adding it to a 2500 ml round bottom flask, heating to 70 C, and stirring the intermediate 91.5 (0.5 mol) for 30 minutes.Rapid cooling to room temperature, and then add hydrochloric acid pH = 5, a white precipitate generated, suction, washing, drying, 5-carboxy cytosine, white powdery solid, 74.9 grams, the yield was 96.8%.
With ammonium chloride; In 1-methyl-pyrrolidin-2-one; at 180℃; for 8h;
Decarboxylation Synthesis of cytosine was carried out by adding 77.5 g (0.5 mol) of intermediate 3, 26.8 g (0.5 mol) of ammonium chloride, 500 ml of N-methylpyrrolidone to a 1000 ml round bottom flask, , Stir the reaction evenly heated to 180C, and heat for 8 hours, heated to reflux until less bubbles removed, stop the reaction, cooled to room temperature, add 150 ml of ether, precipitation solid filtration, collecting white solid is the final product cells Pyrimidine, dried, 49 g of a white crystalline solid in 87% yield.
Stage #1: 5-carboxyl-2′-deoxy-(N1,N3-N)cytidine With hydrogenchloride; water at 20℃; for 48h; Inert atmosphere;
Stage #2: at 45℃; for 15h; Inert atmosphere;
Multi-step reaction with 2 steps
1: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
2: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
Multi-step reaction with 2 steps
1.1: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
2.1: water; hydrogenchloride / 48 h / 20 °C / Inert atmosphere
2.2: 15 h / 45 °C / Inert atmosphere
Multi-step reaction with 3 steps
1.1: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
2.1: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
3.1: water; hydrogenchloride / 48 h / 20 °C / Inert atmosphere
3.2: 15 h / 45 °C / Inert atmosphere
Multi-step reaction with 2 steps
1.1: Ce(4+)*6NO3(1-)*C30H27FeN5O(2+); water / 22 °C / Inert atmosphere
2.1: water; hydrogenchloride / 48 h / 20 °C / Inert atmosphere
2.2: 15 h / 45 °C / Inert atmosphere