Acetone → 1417424-23-7

Participants

Reaction Steps

10 g crude 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride were dissolved in 25 mL water at 70 C. The solution was cooled to 55° C. and 75 mL acetone were added. The mixture was cooled to room temperature within 3 hours and left standing for two days for crystallization. After cooling (4° C.) for 6 hours the product was isolated via filtration, washed with acetone/water (3:1) and dried in vacuum. 7.9 g (purity 97.1%) of 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride dihydrate were obtained. Water content (Karl Fischer): 10.52% b) 8.5 g of crude 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride were dissolved in 21.5 mL water at 65° C. The temperature was lowered to 50° C. in 1 h and 32.3 mL acetone were added in 30 min. The temperature was lowered to 40° C. and the mixture was stirred for 3 h. The reaction mixture was chilled to ambient temperature. The crystalline material was collected, washed with water/acetone (⅓) and dried to yield 4.54 g (purity >99.9%) of 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride dihydrate. Water content (Karl Fischer) 10.6%

Provenance & Evidence