New compound having anti-blood coagulation effect
A compound, C1-C6 technology, applied in the field of medicine
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Embodiment 1
[0061] 5-N-[(1RS)-2-cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl]-4,5,6,7-tetrahydrothiophene[3,2-c Preparation of ]pyridin-2-yl acetylsalicylate
[0062]
[0063] 368 mg of 5-[(1RS)-2-cyclopropyl-1-(2-fluorophenyl 1)-2-oxoethyl]-4,5,6,7-tetrahydrothiophene[3,2 -c] Pyridin-2(4H)-one hydrochloride and 100mg of sodium hydride (52%, dispersed in mineral oil) were added to a 25ml reaction flask, then 2ml of anhydrous tetrahydrofuran was added, stirred for 30 minutes, and then added 200 mg of salicyloyl chloride was stirred and reacted for 2 hours, the reaction was stopped, and 579 mg of a yellowish solid was obtained by column chromatography, with a yield of 11.7%.
[0064] 1 H-NMR (400MHz, CDCl 3 ): δ8.11(d, 1H), 7.58(t, 1H), 7.28(m, 2H), 702-706(m, 2H), 685-691(1n, 2H), 5.45(s, iH), 477(s, 1H), 3.06(t, 2H), 255(t, 2H), 210(s, 3H), 186(m, 2H), 108(m, 1H), 0.55-077(m, 4H) .
[0065] ESI-MS: m / z494 (MH + ).
Embodiment 2
[0067] S(+)-2-(2-chlorophenyl)-2-(2-acetylsalicylate-4,5,6,7-tetrahydrothiophene[3,2-c]pyridine)-5 - Preparation of methyl acetate
[0068]
[0069] 337 mg of S(+)-2-(2-chlorophenyl)-2-(4,5,6,7-tetrahydrothiophene[3,2-c]pyridin-2(4H)-one-5 - Add methyl acetate and 100mg of sodium hydride (52%, dispersed in mineral oil) to a 25ml reaction flask, then add 2ml of anhydrous tetrahydrofuran, stir for 30 minutes, then add 200mg of salicyloyl chloride, continue stirring for 2 hours , the reaction was stopped, and 612 mg of off-white solid was obtained by separation by column chromatography, with a yield of 122%.
[0070] 1 H-NMR (400MHz, CDCl 3 ): δ8.10(d, 1H), 7.55(t, 1H), 7.26(m, 2H), 7.13(m, 1H), 700-706(m, 3H), 685-6.91(m, 2H), 5.45 (s, 1H), 4.77 (s, 1H), 3.68 (s, 3H), 306 (t, 2H), 2.55 (t, 2H), 210 (s, 3H), 1.86 (m, 2H).
[0071] ESI-MS: m / z500 (MH + ).
Embodiment 3
[0073] S(+)-2-(2-chlorophenyl)-2-nicotinate-4,5,6,7-tetrahydrothiophene[3,2-c]pyridine)-5-methyl acetate to prepare
[0074]
[0075] 337 mg of S(+)-2-(2-chlorophenyl)-2-(4,5,6,7-tetrahydrothiophene[3,2-c]pyridin-2(4H)-one-5 - Methyl acetate and 100mg of sodium hydride (52%, dispersed in mineral oil) were added to a 25ml reaction flask, then 2ml of anhydrous tetrahydrofuran was added, after stirring for 30 minutes, 150mg of nicotinoyl chloride was added, and the reaction was continued for 2 hours, The reaction was stopped, and 756 mg of off-white solid was obtained by separation by column chromatography, with a yield of 17.1%.
[0076] 1 H-NMR (400MHz, CDCl 3 ): δ9.12(s, 1H), 8.79(d, 1H), 8.17(d, 1H), 7.49(t, 1H), 715(m, / H), 702-706(m, 3H), 6.85 -691 (m, 2H), 5.48 (s, 1H), 475 (s, 1H), 367 (s, 3H), 306 (t, 2H), 2.53 (t, 2H), 183 (m, 2H).
[0077] ESI-MS: m / z443 (MH + ).
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