Benzothiophene compounds and their preparation and medicine use
A technology of benzothiophenes and compounds, applied in the field of a class of benzothiophenes, their preparation and its medical use, can solve the problems of increasing the risk tendency of deep vein thrombosis
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Embodiment 1
[0044] Example 1 6-methoxy-2-(4-methoxyphenyl)-3-(4-fluoro-benzoyl)-benzothiophene-(Y-69)
[0045] To 1.0 g of 4-fluorobenzoic acid (7.14 mmol) was added 6 ml of redistilled SOCl 2 .1 drop of DME was refluxed for 1 hour. Evaporate the thionyl chloride and drain as much as possible with a water pump. Then add 30mL of dry 1,2-dichloroethane, 1.9 grams of 2-(4-methoxyphenyl)-6-methoxy-benzothiophene (7.03mmol), 3.8 grams of anhydrous trichloro Aluminum chloride (28.5 mmol). React overnight at 5°C-10°C, and quench the reaction with 20 mLTHF. Extract with dichloromethane, combine the organic phases, and dry over anhydrous sodium sulfate. After distilling off the solvent, silica gel column chromatography (petroleum ether / ethyl acetate 15 / 1) gave 2.4 g of yellow powder, with a two-step yield of 86%. NMR (400MHz, CDCl 3 ) δ3.74 (3H, s) 3.89 (3H, s) 6.74 (2H, q, J = 6.8) 6.94 (2H, t, J = 9.0, J = 8.4) 7.0 (1H, dd, J = 9.0, J = 2.4) 7.29 (2H, q, J = 6.8) 7.32 (1H, d, J = 2.4) 7.63 ...
Embodiment 2
[0046] Example 2 6-methoxy-2-(4-methoxyphenyl)-3-[4-(4-benzylpiperazine-)-1-benzoyl]-benzothiophene (Y-66 )
[0047] Dissolve 2.5g of Y-69, 1.8mL of benzylpiperazine, 3mL of triethylamine in dry 10mL of N-methylpyrrolidone, react in an oil bath at 110°C for 20 hours, pour into water, extract with ethyl acetate, anhydrous Na2SO4 dried. After distilling off the solvent, silica gel column chromatography (petroleum ether / ethyl acetate 2 / 1) gave 3.08 g of yellow crystals, with a yield of 88%. NMR (400MHz, CDCl 3 ) δ2.58 (4H, s) 3.33 (4H, s) 3.58 (2H, s) 3.75 (3H, s) 3.87 (3H, s) 6.69 (2H, d, J=9.0) 6.77 (2H, q, J = 2.2, J = 6.6) 6.92 (1H, dd. J = 8.8, J = 2.5) 7.30 ~ 7.35 (6H, m) 7.38 (2H, q, J = 2.2, J = 6.6) 7.46 (1H, d, J =9.0)7.72 (2H,d,J=9.0).
Embodiment 3
[0048] Example 3 6-methoxy-2-(4-methoxyphenyl)-3-[4-(4-piperazinyl)-1-benzoyl]-benzothiophene (Y-68)
[0049] Dissolve 1.5 grams of Y-66 in 20 mL of anhydrous methanol, add 1 gram of ammonium formate and 1 gram of 10% Pd-Cl, reflux for 1.5 hours under nitrogen protection, filter, wash the residue with methanol, evaporate the solvent and then directly perform silica gel column chromatography (two Chloromethane / methanol 25 / 1) gave 0.70 g of a foamy solid. NMR (400MHz, CDCl 3 ) 2.99 (1H, s) 3.01 (4H, t) 3.30 (4H, t) 3.73 (3H, s) 3.86 (3H, s) 6.70 (2H, d, J=9.0) 6.76 (2H, q, J = 2.2, J = 6.9) 6.92 (1H.dd. J = 2.5, J = 8.8) 7.30 (1H, d, J = 2.2) 7.38 (2H, q, J = 2.2, J = 6.9) 7.46 (1H, d , J=8.8) 7.73 (2H,d, J=9.0).
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