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With sulfuric acid; iodine; acetic acid; periodic acid; In water; at 80℃; for 24h;Inert atmosphere;
Mixture of 2-aminopyrimidine (2.4 g, 25 mmol, 1.0 eq.) and elemental iodine (2.7 g, 10.7 mmol, 0.43eq.) was added to 60 ml of glacial acetic acid, and then added periodic acid (0.86 g, 3.76 mmol, 0.15 eq.) and 0.5 ml concentrated sulfuric acid dissolved in sulfuric acid solution 3 ml of water. Place reactions in a nitrogen atmosphere , the reaction was heated to 80 C for 24 hours. The reaction was then poured into a saturated aqueous solution of sodium thiosulfate in until a clear solution, (200 ml × 3) and extracted with dichloromethane, the combined organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure, after column chromatography silica gel to give a white solid 2-amino-5-iodopyrimidine (1.4 g, yield 22.2%).
0.4 g
With iodine; In dimethyl sulfoxide; at 120℃; for 1h;
To a solution of pyrimidin-2-amine (1.0 g, 0.010 mol) in DMSO (10 mL) was added iodine (3.2 g, 0.012 mol). The reaction mixture was stirred at 120C for 1 h. The reaction mass was quenched in water and excess of iodine was neutralised with sodium metabisulphate. The reaction mass was extracted with ethyl acetate and concentrated to afford 0.400 g of the desired product.
EXAMPLE 20 By reacting 2-amino-pyrimidine with 3-carbomethoxy-4-hydroxy-2-methyl-thieno[2,3-e]-1,2-thiazine 1,1-dioxide for 18 hours in a manner analogous to that described in Example 1, there is obtained 4-hydroxy-2-methyl-N-(2-pyrimidinyl)-2H-thieno[2,3-e]-1,2-thiazine-3-carboxamide 1,1-dioxide of decomposition point 221-223 C (recrystallisation from ethanol).
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