反应 #3245936
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04775673
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1-(3-methoxypropionyl) piperazine (6.4 g) and 2-chloro-4-amino-6,7-dimethoxyquinazoline (8.9 g) in 100 ml of isoamylalchohol is refluxed with stirring for 6 hours. The reaction mixture is cooled at room temperature for 12 hours. The crystallized product is separated and wet recrystallized by dissolving in warm methanol, with the subsequent addition of ether to the beginning of turbidity. The yield is 13.4 g of the title compound in the form of a hydrochloride monohydrate, which melts at 268°-272° C. with decomposition. Another crystallization from a methanol-ether mixture yields the analytically pure product melting at 273°-278° C. with decomposition. is refluxed The crystallized product is separated wet recrystallized by dissolving in warm methanol, with the subsequent addition of ether to the beginning of turbidity Another crystallization from a methanol-ether mixture
来源 ID: ord-eb3255d3435c4170859474d863f1e808