反应详情

To a solution of HCl (4M in EtOAc, 40 mL) was added 3-methyl-3-((R)-1-methyl-2-oxo-1,2,3,5-tetrahydro-6-oxa-3,4,10,11b-tetraaza-cyclopenta[b]phenanthren-10-yl)-azetidine-1-carboxylic acid tert-butyl ester (4 g, 9.4 mmol) at 0° C. and the reaction mixture was stirred for 30 min. The resulting precipitate was collected by filtration and recrystallized in EtOH to give (R)-1-Methyl-10-(3-methyl-azetidin-3-yl)-3,5-dihydro-10H-6-oxa-3,4,10,11b-tetraaza-cyclopenta[b]phenanthren-2-one hydrochloride (2.6 g, 85%). 1H NMR (CD3OD, 400 MHz): δ 7.27 (d, J=12.8 Hz, 2H), 6.84 (s, 1H), 6.50 (s, 1H), 5.04 (d, J=6.5 Hz, 1H), 4.79 (m, 2H), 4.62-4.55 (m, 4H), 1.89 (s, 3H), 1.47 (d, J=6.5 Hz, 3H). LC/MS (Table 1, Method 5) Rt=1.988 min; MS m/z: 326 [M+1]+. SFC (Table 1, Method 37) Rt=2.169 min.

1. filtrationThe resulting precipitate was collected by filtration
2. customrecrystallized in EtOH