Water → HCID 86598204, compound

Participants

Reaction Conditions

Reaction Steps

3-Amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridyl)-2-pyrazinecarboxamide 4-oxide (8 g) was dissolved in DMF (80 ml). The solution was cooled to −30° C. To the cooled solution was added phosphoryl chloride (12.7 g) dropwise at −30˜−40° C. After addition of phosphoryl chloride, the temperature of the reaction mixture was raised to −10˜−5° C. The mixture was stirred at −10˜−5° C. for 1 hour. To the reaction mixture was added water (400 ml). The suspension was stirred at 30-35° C. for 15 hours. The pH of the suspension was adjusted to 4.5. The suspension was cooled to 0-5° C. and stirred at the same temperature for 2 hours. The precipitate was collected by filtration and washed with water, and dried in vacuo at 40-50° C., to give 3-amino-5-chloro-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridyl)-2-pyrazinecarboxamide (7.1 g).

Provenance & Evidence