Substituted indolo azaketone compound and preparation method and application thereof
A technology for indoloazepinones and compounds, applied in the field of substituted indoloazepinones and their preparations, capable of solving problems such as adverse reactions, congestion, and digestive disorders in patients with liver and kidney insufficiency
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Embodiment 1
[0062] Example 1. Synthesis of Compound C1
[0063] (1) Synthesis of intermediate M1
[0064]
[0065] Under ice bath, sodium borohydride (57 mg, 1.5 mmol) was slowly added to 10 mL of 7-fluoro-3-(2-nitrovinyl)-1H-indole-4-carboxylic acid methyl ester (264 mg, 1.0 mmol) without Water tetrahydrofuran solution, then slowly drop into 3.0mL of methanol, and react for 1 hour under ice-bath conditions. After the reaction was completed, a saturated ammonium chloride solution was added to quench the reaction, the system was concentrated to remove most of the organic solvent, and then extracted with ethyl acetate, the organic phase was dried with anhydrous sodium sulfate, and separated by column chromatography to obtain intermediate M1 (165 mg). White solid, 62% yield. 1 H NMR (400MHz, CDCl 3 )δ8.56(s,1H),7.84(dd,J=8.4,5.2Hz,1H),7.25(d,J=2.5Hz,1H),6.95(dd,J=9.9,8.5Hz,1H), 4.73 (t, J = 6.5Hz, 2H), 3.96 (s, 3H), 3.71 (t, J = 6.5Hz, 2H).
[0066] (2) Synthesis of Intermediate M2 ...
Embodiment 2
[0075] Example 2. Synthesis of Compound C2
[0076] (1) Synthesis of Intermediate M4
[0077]
[0078] The raw material was replaced by M2 and reacted with 4-chlorobenzyl bromide, and the intermediate M4 was obtained as a white solid according to the method of Example 1, and the yield was 85%. 1 H NMR (400MHz, DMSO-d 6 )δ8.08(t, J=5.7Hz, 1H), 7.68(dd, J=8.4, 4.7Hz, 1H), 7.50(s, 1H), 7.38(d, J=8.4Hz, 2H), 7.15( d,J=8.4Hz,2H),7.01(dd,J=12.4,8.4Hz,1H),5.48(s,2H),3.40(dd,J=9.6,5.4Hz,2H),2.93(s,2H ).
[0079] (2) Synthesis of the final product C2
[0080]
[0081]The raw material was replaced by M4 and reacted in polyphosphoric acid, and the final product C2 was obtained as a white solid with a yield of 40% according to the method of Example 1. Purity: 97%. 1 H NMR (400MHz, DMSO-d 6 )δ11.69(s,1H),7.99(t,J=5.4Hz,1H),7.65(dd,J=8.3,4.8Hz,1H),7.34(d,J=8.3Hz,2H),7.26( d,J=8.3Hz,2H),6.96(dd,J=10.7,8.5Hz,1H),4.07(s,2H),3.39(s,2H),2.85(s,2H). 13 C NMR (126MHz, DMSO-d 6 )δ16...
Embodiment 3
[0082] Example 3. Synthesis of Compound C3
[0083] (1) Synthesis of intermediate M5
[0084]
[0085] The raw material was replaced by M2 to react with 3,4-difluorobenzyl bromide, and the intermediate M5 was obtained as a white solid according to the method of Example 1, and the yield was 85%. 1 H NMR (400MHz, CDCl 3 )δ7.97 (dd, J=8.4, 4.6Hz, 1H), 7.12 (dt, J=10.0, 8.3Hz, 1H), 7.03–6.91 (m, 3H), 6.88 (dd, J=5.2, 3.2Hz , 1H), 6.54 (s, 1H), 5.42 (s, 2H), 3.62 (dd, J=9.8, 5.7Hz, 2H), 3.13–2.97 (m, 2H).
[0086] (2) Synthesis of the final product C3
[0087]
[0088] The raw material was replaced by M5 and reacted in polyphosphoric acid, and the final product C3 was obtained as a white solid with a yield of 30% according to the method of Example 1. Purity: 99%. 1 H NMR (400MHz, CDCl 3 )δ8.49(s,1H),7.93(dd,J=8.0,4.8Hz,1H),7.09(dd,J=18.2,8.4Hz,1H),7.03–6.92(m,2H),6.90(dd , J=6.7, 3.1Hz, 1H), 6.60(s, 1H), 4.07(s, 2H), 3.62(s, 2H), 2.96(s, 2H).
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