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CAS No. : | 1445-39-2 | MDL No. : | MFCD01075666 |
Formula : | C4H4IN3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HAFKCGZQRIIADX-UHFFFAOYSA-N |
M.W : | 221.00 | Pubchem ID : | 241102 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
22.2% | 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. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example 3Synthesis of 5-ethynylpyrimidin-2-amine A flask was charged with <strong>[1445-39-2]5-iodopyrimidin-2-amine</strong> (25.0 g, 110 mmol), acetonitrile (900 ml, 110 mmol), trimethylsilylacetylene (35 ml, 241 mmol), triethylami?e (93 ml, 658 mmol), Pd(PPh3)4CI2 (3.9 g, 5.5 mmol) and finally copper(l) iodide (1.1 g, 5.5 mmol). The flask was put under vacuum then filled with argon and stirred at RT overnight using a mechanical stirrer. The solvent was removed under vacuum, the residue taken up in methanol (600ml) and potassium carbonate (152 g, 1097 mmol) was added. The mixture was stirred at RT using mechanical stirring for 2 hrs. Activated carbon (~50ml_) was added to the reaction and stirring continued for 15min. The reaction mixture was then filtered through a plug of celite and the filtrate was concentrated to a volume of ~400mL and the precipitate was filtered. The filtrate was concentrated down to a thick paste which was slurried in ~150mL of 10%MeOH/H2O for 20 min at RT. The solids were then filtered off to afford 5-ethynylpyrimidin-2-amine. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
23% | With pyridine; at 110℃; for 48h; | Step 1: N- (5-LODOPYRIMIDIN-2-YL) acetamide (248) [0400] 5-lodo-pyrimidin-2-ylamine (17,1. 1 g, 4.98 MMOL) and acetic anhydride (14.94 MMOL, 1.41 mL) were dissolved in pyridine (20 mL) and stirred at 110C for 48 hours. The reaction mixture was cooled and quenched with water (50 mL). Ethyl acetate (100 mL) was added and the resulting white precipitate was collected by filtration to afford title compound 248 as a white solid (300 mg, 23% yield NMR: (DMSO) 8 10.67 (s, 1H), 8.85 (s, 2H), 2.18 (s, 3H). |
[ 514854-13-8 ]
6-Ethyl-5-iodopyrimidine-2,4-diamine
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