反应详情

N-butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide (limiting reagent) was dissolved in EtOH (15 vols) and 4.9M sulphuric acid (1 molar equivalent) was added and the solution was stirred at room temp for 48 hours. The precipitate was collected, washed with EtOH (1 vol) and vacuum dried (oven at 40° C., oil pump) to leave a white solid (70% recovery). 5% water in MeCN (20 volumes) was added and the mixture stirred for 6 days. Crystalline solid (form G) was then collect by filtration (95% recovery).

1. customThe precipitate was collected
2. washwashed with EtOH (1 vol) and vacuum
3. customdried (oven at 40° C., oil pump)
4. customto leave a white solid (70% recovery)
5. stirringthe mixture stirred for 6 days
6. filtrationCrystalline solid (form G) was then collect by filtration (95% recovery)