Hydrochloric Acid → HCID 57635042, compound

Participants

Reaction Steps

A mixture of 0.23 g (0.00085 mole) of 4-(9-cyclobutyl-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide (I-24) and 3 mL of 1M hydrochloric acid was heated at 180 degree for 45 minutes in a microwave reactor. The cooled mixture was diluted with 2 mL of water, 3 mL of methanol and 2 mL of acetonitrile and then stirred for 15 minutes. The solids were removed by filtration and the aqueous solution was made basic (pH>10). The solid which formed was collected, washed with water, and then purified by C18 reverse phase silica gel chromatography, eluting with an acetonitrile-water gradient (10:90-100:0) to give 0.037 g of 9-cyclobutyl-2-(2-methoxy-phenylamino)-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (I-25)

Provenance & Evidence