A kind of o-quinone compound and its preparation method and medical application
A compound, o-quinone technology, applied in the application field of preparation of medicines, can solve the problems of weak curative effect, large toxic and side effects, etc.
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Embodiment 1
[0093] Example 1: (E)-3-(pyridin-3-yl)-N-(4-(((1,6,6-trimethyl-10,11-dione-6,7,8,9 Synthesis of ,10,11-hexahydrophenanthrene[1,2-b]furan-2-yl)methyl)amino)phenyl)acrylamide
[0094]
[0095] Step 1: Synthesis of (E)-N-(4aminophenyl)-3-(pyridin-3-yl)acrylamide hydrochloride (6a)
[0096]Weigh (E)-3-(3-pyridine)acrylic acid 3 (500 mg, 3.35 mmol), dissolve it in anhydrous DMF (10 mL), add HATU (1.9 g, 5.03 mmol), DIPEA (10.05 mmol, 1.3 g in turn) ) and N-BOC-p-phenylenediamine 4a (697.7 mg, 3.35 mmol), the reaction was stirred at room temperature for 2 h, the reaction was stopped, and DMF was spin-dried under reduced pressure. To the reaction residue was added 5 ml of saturated NaHCO 3 solution, DCM (20ml×3), combined organic phases, saturated NH 4 Washed once with Cl (10ml), washed once with saturated brine (10ml), dried over anhydrous sodium sulfate, filtered, evaporated to dryness, made sand, separated and purified by column chromatography (DCM:MeOH=60:1~20:1 ) to give ...
Embodiment 2
[0103] Example 2: (E)-3-(pyridin-3-yl)-N-(4-(1-((1,6,6-trimethyl-10,11-dione-6,7,8 Synthesis of ,9,10,11-hexahydrophenanthrene[1,2-b]furan-2-yl)methyl)piperidin-4-yl)phenyl)acrylamide (S2)
[0104]
[0105] 1 H NMR (300MHz, DMSO-d 6 )δ10.22(s, 1H), 8.81(s, 1H), 8.58(d, J=4.7Hz, 1H), 8.03(d, J=8.0Hz, 1H), 7.79(d, J=8.2Hz, 1H), 7.75–7.53 (m, 4H), 7.48 (dd, J=8.0, 4.8Hz, 1H), 7.20 (d, J=8.2Hz, 2H), 6.91 (d, J=15.8Hz, 1H), 3.60(s, 2H), 3.10–3.02(m, 2H), 2.98(d, J=10.5Hz, 2H), 2.41(d, J=11.9Hz, 1H), 2.19(s, 3H), 2.14(d , J=10.9Hz, 2H), 1.84–1.67 (m, 4H), 1.67–1.55 (m, 4H), 1.28 (s, 6H). 13 C NMR (126MHz, Chloroform-d) δ: 183.8, 176.0, 163.4, 161.0, 150.6, 150.3, 149.3, 144.6, 142.5, 138.5, 136.3, 134.7, 133.9, 130.8, 127.5, 127.5, 126.6, 120.73.9, ,120.5,120.4,119.3,54.0,52.6,41.9,38.0,34.8,33.4,32.0,30.1,19.3,9.2.ESI-HRMS m / z calculated for C 39 H 40 N 3 O 4 [M+H] + 614.30133, found 614.30093.
Embodiment 3
[0106] Example 3: (E)-3-(pyridin-3-yl)-N-(4-((2-(((1,6,6-trimethyl-10,11-dione-6,7 ,8,9,10,11-Hexahydrophenanthrene[1,2-b]furan-2-yl)methyl)amino)ethyl)amino)phenyl)acrylamide (S3)
[0107]
[0108] 1 H NMR (300MHz, DMSO-d 6 )δ: 8.75(d, J=2.1Hz, 1H), 8.62–8.45(m, 1H), 8.22(t, J=5.7Hz, 1H), 8.00(d, J=8.0Hz, 1H), 7.76( d, J=8.2Hz, 1H), 7.52–7.39 (m, 3H), 6.99 (d, J=8.0Hz, 2H), 6.73 (d, J=15.9Hz, 1H), 6.64 (d, J=8.1 Hz, 2H), 4.27(s, 2H), 3.38–3.25(m, 2H), 3.02(d, J=6.5Hz, 2H), 2.62(t, J=7.5Hz, 2H), 2.20(s, 3H) ), 1.75–1.64(m, 2H), 1.63–1.53(m, 2H), 1.26(s, 6H). 13 C NMR (126MHz, DMSO-d 6 )δ: 182.4, 175.0, 164.3, 159.0, 151.7, 149.5, 149.2, 148.6, 148.5, 146.4, 142.8, 134.9, 134.5, 134.4, 133.4, 131.0, 129.1, 127.2, 126.6, 124.5, 124.4, 124. ,120.0,119.8,116.2,112.6,40.7,38.0,37.4,34.3,34.2,31.5,29.5,18.7,8.5.ESI-HRMS m / z calculated for C 36 H 36 N 3 O 4 [M+H] + 574.27003, found 574.26959.
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