Ligustrazine-based chalcone-containing aryloxyalkanoic acid compound, preparation method and application thereof
A compound and composition technology, applied in the field of treating hyperlipidemia, atherosclerosis, containing ligustrazine-based chalcone aryloxyalkanoic acid compounds, can solve problems such as liver damage and high price
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Embodiment 1
[0032] Synthesis of (E)-2-ethyl-(4-(3-(3,5,6-trimethylpyrazin-2-yl)acryloyl)phenoxy)acetate (YA1) Preparation 1.12 Synthesis of -Hydroxymethyl-3,5,6-trimethylpyrazine
[0033]
[0034] reaction steps
[0035] In the 250mL three-necked flask, add ligustrazine (15.0g, 0.1mol) successively, 30%H 2 o 2 Solution (24mL, 0.2mol), 15mL of glacial acetic acid, reacted at 94°C for 12h, TLC (petroleum ether-ethyl acetate 1:1) detected that the reaction was almost complete, adjusted the pH to 10 with 50% NaOH solution under cooling, dichloro Extract with methane (3×30mL), combine the organic phases, wash over anhydrous Na 2 SO 4 After drying, it was concentrated under reduced pressure to obtain 13.2 g of white crystals of ligustrazine mononitrogen oxide, yield 78.8%, mp 82.4-84.1°C.
[0036] Ligustrazine mononitrogen oxide (13.2g, 86.8mmol) and acetic anhydride (31.2mL, 330.4mmol) were sequentially added into a 250mL three-necked flask, reacted at 130°C for 5h, and detected by TLC...
Embodiment 2
[0051] Synthesis of (E)-2-ethyl(3-(3-(3,5,6-trimethylpyrazin-2-yl)acryloyl)phenoxy)ethyl ester (YA2)
[0052]
[0053] Reaction steps: the synthesis of 3,5,6-trimethylpyrazine-2-carbaldehyde was synthesized according to the method 1.1 and 1.2 in Example 1, and the operation was carried out according to the method 1.3 and 1.4 in Example 1 to obtain YA2 light yellow crystal, m.p.116.1 -116.9°C. 1 H NMR (300MHz, CDCl 3 )δ:8.19(d,J=14.7Hz,1H,=CH),8.00(d,J=14.7Hz,1H,=CH),7.77(d,J=7.5Hz,1H,PhH),7.62(s ,1H,PhH),7.45(t,J=7.8Hz,1H,PhH),7.18(dd,J=2.4Hz,8.1Hz,1H,PhH),4.72(s,2H,OCH 2 CO), 4.30 (q, J=7.2Hz, 2H, OCH 2 CH 3 ),2.66(s,3H,CH 3 ),2.57(s,3H,CH 3 ),2.55(s,3H,CH 3 ), 1.32(t, J=7.2Hz, 3H, OCH 2 CH 3 ); 13 C NMR (CDCl 3 ,75MHz)δ:189.5,168.5,158.1,152.8,149.9,149.6,142.9,139.3,138.5,129.8,126.1,122.3,120.0,113.9,65.4,61.5,22.1,21.8,20.8,14.2cm; IR(KBr, -1 )υ: 3067.9, 2981.5, 2914.2, 1742.1, 1658.7, 1585.7, 1482.6, 1450.5, 1437.5, 1398.4, 1211.7, 1186.2, 1085.2, 966.9, 8...
Embodiment 3
[0055] Synthesis of (E)-ethyl-2-methyl-2-(4-(3-(3,5,6-trimethylpyrazin-2-yl)acryloyl)phenoxy)propionate ( YA3)
[0056]
[0057] Reaction steps: the synthesis of 3,5,6-trimethylpyrazine-2-carbaldehyde is synthesized according to the method 1.1 and 1.2 in Example 1, and is operated according to the method 1.3 and 1.4 in Example 1 to obtain (E)-ethyl- 2-Methyl-2-(4-(3-(3,5,6-trimethylpyrazin-2-yl)acryloyl)phenoxy)propionate Yellow crystals, m.p.122.8-123.3°C. 1 H NMR (300MHz, CDCl 3 )δ: 8.13 (d, J = 14.7Hz, 1H, = CH), 8.00 (d, J = 8.7Hz, 2H, PhH), 7.91 (d, J = 14.7Hz, 1H, = CH), 6.83 (d ,J=8.7Hz,2H,PhH),4.16(q,J=7.2Hz,2H,OCH 2 CH 3 ),2.58(s,3H,CH 3 ),2.48(s,3H,CH 3 ),2.47(s,3H,CH 3 ),1.60(s,6H,2×CH 3 ), 1.15(t, J=7.2Hz, 3H, OCH 2 CH 3 ); 13 C NMR (CDCl 3 ,75MHz)δ:188.4,173.7,159.9,152.6,149.8,149.6,143.2,137.6,131.4,130.6,126.1,117.4,79.3,61.7,25.4,22.0,21.8,20.8,14.0; IR(KBr,cm -1 )υ: 3045.6, 2997.5, 2949.5, 1731.8, 1656.5, 1605.6, 1588.6, 1508.2, 1326.9, 1277.0...
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