ChemicalBook CAS DataBase List 2-Cyanopyrimidine

2-Cyanopyrimidine synthesis

13synthesis methods

Product Name:2-Cyanopyrimidine
CAS Number:14080-23-0
Molecular formula:C5H3N3
Molecular Weight:105.1

773837-37-9 Synthesis

773837-37-9
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14161-09-2 Synthesis

14161-09-2
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14080-23-0
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Yield:14080-23-0 16.3 g

Reaction Conditions:

in water;acetonitrile at 18 - 22;

Steps:

1.S2-3.S2; 1.S3-3.S3 S2, cyano substitution reaction:

Add acetonitrile (255mL) to the reaction solution in the above-mentioned three-necked flask, and stir for 15min;Take sodium cyanide (12.8g), dissolve the sodium cyanide with water (25mL) ultrasonically, then drop it into the reaction solution, after the dripping, add water (4mL) to the there-necked bottle,Stir overnight at room temperature (18-22°C);On the fourth day, spotting showed that the raw material (2-thiamphenicol pyrimidine) disappeared and 2-cyanopyrimidine was generated.S3, follow-up processing:The temperature of the reaction solution in the three-neck flask was raised to 25°C, concentrated under reduced pressure to recover acetonitrile (vacuum degree less than -0.090MPa, water pump decompression, circulating condensed water temperature 0-10°C) for about 1.5h, and then added ethyl acetate (250mL ) and water (50mL), stirred for 10min, filtered, the filter cake was washed twice with ethyl acetate, and drained, the combined filtrate was extracted, the aqueous layer was extracted once again with ethyl acetate (150mL), and the organic layers were combined. Washed twice with 10% aqueous sodium chloride (200 mL), dried over anhydrous sodium sulfate, filtered, spin-dried, and separated with methanol (100 mL), strip-dried again to give 2-cyanopyrimidine (16.3 g), LC purity : 97.1%, two-step yield: 76.7%.The extracted water layers were combined, and the filtered filter cake was soaked and reacted overnight with 10% sodium hypochlorite aqueous solution (500 mL) for harmless treatment.

References:

CN115215805,2022,A Location in patent:Paragraph 0047-0050; 0055-0065; 0070-0080; 0085-0091

1722-12-9 Synthesis