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2H-1,4-Benzodiazepin-2-one, 3-amino-9-fluoro-1,3-dihydro-5-phenyl- synthesis
- Product Name:2H-1,4-Benzodiazepin-2-one, 3-amino-9-fluoro-1,3-dihydro-5-phenyl-
- CAS Number:1584714-99-7
- Molecular formula:C15H12FN3O
- Molecular Weight:269.27
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1584715-01-4
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Yield:1584714-99-7 95%
Reaction Conditions:
with hydrogen bromide;acetic acid at 20; for 1.5 h;
Steps:
B1 Intermediate B 1
A mixture oflntermediate BIA (9 g, 22.31 mmol) in 33% HBr in HOAc (29.4ml, 178 mmol) was stirred at room temperature for 1.5h. Ether was added, then theprecipitate was collected by filtration and rinsed with ether. The solid was suspended inwater (150 mL) and saturated NaHC03 was added while stirring. The solid was collected by filtration, rinsed with water, and dried under vacuum to give Intermediate B1 (5.69g,95%): HPLC: RT= 1.227 min (H20/MeOH with TFA, CHROMOLITH SpeedROD,4.6x50mm, gradient= 4 min, wavelength= 220 nm); MS(ES): m/z = 270 [M+H+]; 1HNMR (400 MHz, DMSO-d6) 8 10.57 (br. s., 1H), 7.61-7.36 (m, 6H), 7.32-7.19 (m, 1H),5 7.11 (d, J=7.9 Hz, 1H), 4.34 (s, 1H), 2.76-2.55 (m, 2H).
References:
WO2014/47374,2014,A1 Location in patent:Paragraph 00286
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1584139-76-3
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317-20-4
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![PHENYLMAGNESIUM BROMIDE](/CAS/GIF/100-58-3.gif)
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