Related Products of 39095-25-5,Some common heterocyclic compound, 39095-25-5, name is 2,5-Dimethylterephthalonitrile, molecular formula is C10H8N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In 100ml 4-neck reactor 2,5-dimethyl-terephthalonitrile 2.3g, Carbon tetrachloride 23ml, NBS 5.3g, AIBN 0.07g 1 hour reaction at charged 75C It was. After completion of the reaction, it was allowed to cool to room temperature. Wash the residue and the reaction solution was filtered with carbon tetrachloride It was. Crude product is obtained in the oil and the filtrate was concentrated. The addition of methanol and allowed to crystallize the crude product. Taken out crystals were filtered off, 1,4-dicyano-2,5-bis-bromo methyl benzene was obtained 0.57g. In 50ml 3-necked reactor 1,4-dicyano-2,5-bis bromomethylbenzene 0.55g, Triethyl phosphite 0.61g was stirred and heated to charged 100-110 . At this temperature the reaction was carried out for 2 hours. Was allowed to cool to room temperature, and purified on a silica gel column 2,5-dicyano-1,4-bis (diethyl phosphonyl methyl) benzene was obtained 0.45g. 50ml 3-necked reactor to 2,5-dicyano-1,4-bis (diethyl phosphonyl methyl) benzene 0.45g, DMF (dehydration) 15ml, 4 formylpyridine 0.28g They were charged. After nitrogen substitution, Potassium t- butoxide 0.35g It was changed to green-brown solution and dropping the 5mlDMF solution slowly. It was allowed to react for 3 hours at 60 . The reaction mixture was extracted with chloroform and released into the water. The reaction mixture was concentrated to give crude product. The crude product was purified on a silica gel column (toluene / acetone 1/1) and the resulting solid to yield 0.08g of intermediate 45 and purified construed methanol. A synthesis flow of this intermediate 45 below
The synthetic route of 39095-25-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; RICOH COMPANY LIMITED; YAMADA CHEMICAL COMPANY LIMITED; HIRANO, SHIGENOBU; YASHIRO, TOHRU; MANABE, YOUSUKE; HAYASHI, SATOSHI; (35 pag.)JP5900813; (2016); B2;,
Nitrile – Wikipedia,
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