Fluoroalkyl and fluorocycloalkyl 1,4-benzodiazepinone compounds as notch inhibitors
A technology of benzodiazepines and compounds, applied in the field of pharmaceutical compositions, capable of solving problems such as tumor formation
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Embodiment 1
[0499] (2R,3S)-3-((3,3-difluorocyclobutyl)methyl)-N-((3S)-9-methyl-2-oxo-5-phenyl-2,3- Dihydro-1H-1,4-benzodiazepine -3-yl)-2-(3,3,3-trifluoropropyl)succinamide
[0500]
[0501] Example 1A: (2S,3R)-2-((3,3-difluorocyclobutyl)methyl)-6,6,6-trifluoro-3-(((S)-9-methyl- 2-Oxo-5-phenyl-2,3-dihydro-1H-benzo[e][1,4]diazepine -3-yl)carbamoyl)hexanoic acid tert-butyl ester
[0502]
[0503] To a solution of Intermediate B-1,2 hydrobromide (308 mg, 0.721 mmol), Intermediate S-1 (225 mg, 0.601 mmol) and TBTU (289 mg, 0.902 mmol) in DMF (4 mL) was added TEA ( 0.335 mL, 2.404 mmol). The mixture was stirred at room temperature for 50 min. Add NaHCO 3 dilution while stirring. The resulting solid was collected by filtration, rinsed with water, dried, and purified by silica gel chromatography (12g column, EtOAc / Hexane = 0-70%) to give Example 1A (327 mg, 99% yield). HPLC: RT=3.400min (H 2 O / MeOH with TFA, SpeedROD, 4.6x50mm, gradient=4min, wavelength=220nm) MS(ES): m / z=622[...
Embodiment 2
[0507] (2R,3S)-3-(4,4-difluorocyclohexyl)-N-((3S)-9-methoxy-2-oxo-5-phenyl-2,3-dihydro-1H -1,4-Benzodiazepine -3-yl)-2-(3,3,3-trifluoropropyl)succinamide
[0508]
[0509] Example 2 was prepared from Intermediate B-2 and Intermediate S-3 according to the general procedure shown in Example 1. Example 2 was obtained. HPLC: RT=10.27min (H 2 O / CH 3 CN, containing TFA, SunFire C18 3.5μm, 4.6x150mm, gradient=15min, wavelength=220and 254nm); MS(ES):m / z=595[M+H + ]; 1 H NMR (400MHz, methanol-d 4 )δ10.08(s,1H),9.48(d,J=7.5Hz,1H),7.60-7.42(m,5H),7.38-7.19(m,2H),6.96(br.s.,1H), 6.92-6.83(m,1H),5.27(d,J=7.5Hz,1H),3.94(s,2H),3.05-2.89(m,1H),2.57(d,J=5.1Hz,1H),2.31 -2.19 (m, 1H), 2.10-1.90 (m, 3H), 1.87-1.75 (m, 1H), 1.73-1.41 (m, 5H), 1.37-1.22 (m, 1H).
Embodiment 3
[0511] (2R,3S)-N-((3S)-9-(cyclopropyloxy)-5-(3-fluorophenyl)-2-oxo-2,3-dihydro-1H-1,4 - Benzodiazepines -3-yl)-3-(4,4-difluorocyclohexyl)-2-(3,3,3-trifluoropropyl)succinamide
[0512]
[0513]Example 3 was prepared according to the general procedure shown in Example 1 from Intermediate B-6 and Intermediate S-3. The solid was chromatographed by preparative SFC (Welk O(RR) 250x 30mm ID, 5 μm, 84 / 16CO 2 / MeOH, 120mL / min) to obtain Example 3. HPLC: RT=10.95min (H 2 O / CH 3 CN with TFA, SunFire C18 3.5μm, 4.6x150mm, gradient = 15min, wavelength = 220 and 254nm); MS (ES): m / z = 639 [M+H + ]; 1 H NMR (400MHz, methanol-d 4 )δ10.05(s,1H),9.47(d,J=7.3Hz,1H),7.60(dd,J=8.3,1.2Hz,1H),7.55-7.45(m,2H),7.44-7.24(m ,4H),6.94(dd,J=7.9,1.1Hz,2H),5.27(d,J=7.3Hz,1H),4.03(tt,J=5.9,2.9Hz,1H),3.05-2.91(m, 1H),2.32-2.17(m,1H),2.00(d,J=12.1Hz,4H),1.77-1.41(m,8H),1.38-1.20(m,2H),0.99-0.92(m,1H) ,0.90-0.81(m,2H),0.80-0.67(m,1H).
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