Hydrochloric Acid → HCID 86731036, compound

Participants

Reaction Steps

To a mixture of 1-{[(4aR,6R,8aR)-2-amino-3-cyano-8-methyl-4H,4aH,5H,6H, 7H,8H,8aH,9H-thieno[3,2-g]quinolin-6-yl]carbonyl}-3-[(2S)-1-(dimethylamino)propan-2-yl]-1-ethylurea (compound 1-57) (0.88 g) and 2-propanol (17.6 mL) was added 12 mol/L hydrochloric acid (0.36 mL) while stirring under water bath cooling. To the solution was added dropwise diisopropyl ether (17.6 mL), and stirred at the room temperature for 1 hour, then for 1 hour under ice bath cooling. The resulting solid was collected by filtration, and washed twice with ice-cold 2-propanol/diisopropyl ether mixed solvent (2-propanol:diisopropyl ether=1:1) (4.4 mL) to give 1-{[(4aR,6R,8aR)-2-amino-3-cyano-8-methyl-4H,4aH,5H,6H,7H,8H,8aH,9H-thieno-[3,2-g]quinolin-6-yl]carbonyl}-3-[(2S)-1-(dimethylamino)propan-2-yl]-1-ethylurea di hydrochloride salt (0.92 g).

Provenance & Evidence