Warfarin-4-O-acetyl-Gly-Pro-Arg-Pro-AA1 as well as synthesis, activity and application thereof
A -gly-pro, warfarin technology, applied in the directions of active ingredients of heterocyclic compounds, medical preparations of non-active ingredients, drug combinations, etc., can solve problems such as large bleeding side effects due to dose differences
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Embodiment 1
[0022] Embodiment 1 prepares warfarin-4-O-benzyl acetate (1)
[0023] Disperse 26.48g (80.00mmol) warfarin in 400mL acetone, stir at 45°C until the warfarin dissolves, add 12.1g (88.0mmol) K 2 CO 3 , then add 14mL (88mmol) benzyl bromoacetate, continue to stir at 45°C for 96 hours, TLC (petroleum ether / ethyl acetate, 2 / 1) shows that the raw material point disappears, filter, and concentrate the filtrate under reduced pressure to obtain a light yellow oil The compound was purified by silica gel column chromatography (petroleum ether / ethyl acetate, 8 / 1) to obtain 19.77 g (54%) of the title compound as a colorless solid. ESI-MS(m / e):457[M+H] + ; 1 H NMR (300MHz, DMSO-d 6 )δ / ppm=7.89(dd,J 1 =3.0Hz,J 2 =9.0Hz,1H),7.63(dt,J 1 =3.0Hz,J 2 =9.0Hz, 1H), 7.43~7.31(m, 9H), 7.24(t, J=9.0Hz, 2H), 7.15(tt, J=9.0Hz, 1H), 5.26(s, 2H), 5.61(s ,1H),5.02(d,J=15.0Hz,1H),4.85(d,J=15.0Hz,1H),4.97(t,J=9.0Hz,1H),3.45(dq,J 1 =9.0Hz,J 2 =18.0Hz, 2H), 2.11(s, 3H).
Embodiment 2
[0024] Embodiment 2 prepares warfarin-4-O-acetic acid (2)
[0025] Dissolve 19.77g (43.36mmol) of warfarin-4-O-benzyl acetate (1) in 150mL of tetrahydrofuran, add 4.94g of Pd / C and stir, remove the air, introduce hydrogen, and stir at room temperature for 72 hours. TLC (petroleum ether / ethyl acetate, 2 / 1) showed that the raw material point disappeared. After filtration, the filtrate was concentrated under reduced pressure to obtain 15.58 g (98.%) of the title compound as a colorless solid. ESI-MS(m / e):367[M+H] + ; 1 H-NMR (300MHz, DMSO-d 6):δ / ppm=12.86(s,1H),7.90(d,J=6.0Hz,1H),7.63(t,J=6.0Hz,1H),7.43~7.34(m,4H),7.27(t, J=9.0Hz, 2H), 7.17(t, J=9.0Hz, 1H), 4.99(t, J=9.0Hz, 1H), 4.75(dd, J 1 =15.0Hz,J 2 =30.0Hz, 2H), 3.54~3.47(m, 2H), 2.14(s, 3H).
Embodiment 3
[0026] Embodiment 3 prepares Boc-Gly-Pro-OBzl
[0027] Dissolve 7.730g (44.15mmol) Boc-Gly in 100mL dry tetrahydrofuran, add 5.940g (44.00mmol) 1-hydroxybenzotriazole and 9.888g (48.00mmol) dicyclohexylcarbodiimide at 0°C, stir 30 minutes. Add 9.665g (40.00mmol) HCl Pro-OBzl to the reaction solution at 0°C, adjust the pH value of the reaction solution to 9 with N-methylmorpholine, stir at room temperature for 17 hours, TLC (dichloromethane / methanol, 20 / 1) It shows that the raw material point disappears, filter, concentrate the filtrate under reduced pressure, dissolve the residue with 150mL ethyl acetate, filter, and use saturated NaHCO 3 Wash with aqueous solution (50mL×3), wash with saturated NaCl aqueous solution (50mL×3), 5% KHSO 4 Wash with aqueous solution (50mL×3), wash with saturated NaCl aqueous solution (50mL×3), and wash with saturated NaHCO 3 Wash with aqueous solution (50mL×3), wash with saturated NaCl aqueous solution (50mL×3), dry the ethyl acetate phase wit...
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