3-Methylxanthine synthesis
- Product Name:3-Methylxanthine
- CAS Number:1076-22-8
- Molecular formula:C6H6N4O2
- Molecular Weight:166.14
90801-87-9
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1076-22-8
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Yield:1076-22-8 95.12%
Reaction Conditions:
with formic acid;perchloric acid adsorbed on silica gel in ethanol at 20; for 0.333333 h;Solvent;
Steps:
7-10 Example 7
Add 12.61g (0.09mol, M=140.15) of 4-(methylamino)-1H-imidazole-5-carboxamide (3) and 60ml of absolute ethanol in a round bottom flask, stir to dissolve, add to the constant pressure funnel and add 8.26g of anhydrous formic acid (0.12mol, M=68.9), add 0.38g of catalyst HClO4-SiO2, slowly drip the solution in the constant pressure funnel into the reaction flask, reaction time at room temperature 20min, TLC monitoring until the reaction is complete, add 40 % Sodium hydroxide aqueous solution was adjusted to neutral or weakly acidic, filtered to obtain the filtrate, solid recovery, ice-bath cooling charge analysis to determine the solid, washed with ice ethanol, vacuum dried to obtain compound 4, 14.22g, yield 95.12%, purity 99.9% , The maximum single miscellaneous is 0.01%.
References:
CN112679500,2021,A Location in patent:Paragraph 0049-0057
64-18-6
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1076-22-8
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