3-Chloropyrazine-2-carbonitrile synthesis

10synthesis methods

Product Name:3-Chloropyrazine-2-carbonitrile
CAS Number:55557-52-3
Molecular formula:C5H2ClN3
Molecular Weight:139.54

55321-99-8 Synthesis

55321-99-8
198 suppliers
$35.39/250mg

55557-52-3
254 suppliers
$12.00/5g

Yield:55557-52-3 79%

Reaction Conditions:

with N-ethyl-N,N-diisopropylamine;trichlorophosphate in chlorobenzene at 0 - 90;

Steps:

1-1 Step 1: Synthesis of Preparation of 3-chloro-pyrazine-2-carbonitrile
At 0 , a solution of 3-hydroxy-2-carboxamide (5g, 37mmol) in chlorobenzene (20 mL) was added dropwise phosphorus oxychloride (2mL, 40mmol) and diisopropylethylamine (3.5mL, 80mmol), dropwise addition, the reaction mixture was stirred overnight at 90 placed.After the reaction, the reaction solution was concentrated under reduced pressure the reaction solution, the residue was diluted with 20mL water, (20mL x 3) and extracted with EtOAc, the combined organic phases were dried over anhydrous sodium sulfate, and then concentrated under reduced pressure, the residue was purified by silica gel column chromatography ( eluant: PE / EtOAc (V / V) = 10/1) to give the title compound as a white solid (4.5g, 79%).

References:

Guangdong East Sunshine Pharmaceutical Co., Ltd.;Reng, Qingyun;Liu, Xinchang;Tang, Changhua;Zhang, Jiancun;Zhang, Yingjun CN104447584, 2016, B Location in patent:Paragraph 0138; 0139; 0140

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