Application of 1256825-86-1, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 1256825-86-1 as follows.
Bromine oxidation reaction:With 5 liters three bottles,Under mechanical agitation,60 g of 7-azaindole-6-carboxylic acid methyl ester,After adding 3.7 liters of tert-butanol,When the temperature was raised to 40 C,545 g of pyridine hydrobromide perbromide(PBPB) were added portionwise,At the end of 1 hour.And then kept at 40 C for 1 hour.Sampling monitoring,HPLC showed a starting material / product ratio of no more than 1%. Post-treatment and recrystallization:The reaction solution was poured into 5 liters of ice water, extracted with ethyl acetate (5 liters) at a temperature of 5 C, and the organic layer was collected.The mixture was concentrated to a volume of 1/3 solvent and poured into 3 liters of ice water. The solid was precipitated, filtered and the cake was washed with 500 ml of water and dried. Recrystallization was carried out using a 1: 5 weight ratio of ethyl acetate to methanol,Filtration,After drying under reduced pressure,Methyl 3,3-dibromo-2-oxo-7-azaindole-6-carboxylate (3), 85 g was obtained and sampled and HPLC showed a purity of 90%
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1256825-86-1, its application will become more common.
Reference:
Patent; SUZHOU HEJIAN MEDICAL TECHNOLOGY CO LTD; SHANG, XINJUN; LI, JIAHE; (8 pag.)CN104387385; (2016); B;,
Pyridine – Wikipedia,
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