Thrombase inhibitor containing guanidyl heterocyclic compound and preparation method thereof
A technology of thrombin inhibitors and heterocyclic compounds, which is applied in the field of chemical synthesis, can solve the problems of low yields of synthetic key intermediate compounds, achieve the effects of inhibiting thrombin production, simple operation and separation, and high yields
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Embodiment 1
[0068] When R 1 When it is 2-pyridine,
[0069] Synthesis of 3-({2-[(4-cyano-phenylimine)-methylene]-1-methylene-1hydro-benzimidazole-5-carbonyl}-pyridine-2-imine)- Ethyl propionate (1)
[0070] Compound 2-(4-cyano-phenylamino)-acetic acid (2.32g, 13.2mmol) was dissolved in 80ml DMF, HOBT (1.96g, 14.5mmol) was added, and EDCI (2.77g, 14.5mmol) was added below 0°C ) stirred for 10-60min, slowly rose to room temperature, added diamine compound 3-(N,N-(2-pyridine)-[3-amino-4-methylamino-benzoyl]-propionic acid ethyl ester (5.0 g, 14.5mmol).Reacted for 2~6h, concentrated, diluted with a large amount of ethyl acetate, washed three times with saturated brine, and washed with Na 2 SO 4 After drying and concentration, the crude product was refluxed in 60ml of acetic acid for 1.5h. After concentration, it was basified and extracted with ethyl acetate (60mL×3) three times. The organic phase was washed once with saturated brine, washed with Na 2 SO 4 After drying and concentration,...
Embodiment 2
[0085] When R 1 For 2-pyridine:
[0086] Synthesis of 3-({2-[(4-nitro-phenylimine)-methylene]-1-methylene-1hydro-benzimidazole-5-carbonyl}-pyridine-2-imine)- Ethyl propionate (7)
[0087] Compound 2-(4-nitro-phenylamino)-acetic acid (3.14g, 15.95mmol) was dissolved in 20ml DMF, HOBT (2.40g, 17.54mmol) was added, and EDCI (3.35g, 17.54mmol) was added below 0°C ) stirred for 5-60min, slowly rose to room temperature, added diamine compound 3-(N,N-(2-pyridine)-[3-amino-4-methylamino-benzoyl]-propionic acid ethyl ester (6.0 g, 17.54mmol).Reacted for 2~6h, concentrated, diluted with a large amount of ethyl acetate, washed three times with saturated brine, and washed with Na 2 SO 4 After drying and concentration, the crude product was refluxed in 30ml of acetic acid for 1.5h, after concentration, it was basified, extracted with ethyl acetate (30mL×3) three times, the organic phase was washed once with saturated brine, washed with Na 2 SO 4 After drying and concentration, the crud...
Embodiment 3
[0099] When R 1 For 4-fluoro-phenyl,
[0100] Synthesis of 3-({2-[(4-methylguanidino-phenylimine)-methylene]-1-methylene-1hydro-benzimidazole-5-carbonyl}-4-fluorophenyl- 2-imino)-propionic acid
[0101] The synthetic method is as embodiment 1,
[0102] 1 H NMRδ (300MHz, DMSO-d 6 ): 7.87(m, 1H), 7.54-7.49(m, 2H), 7.29-7.24(m, 4H), 7.11-7.04(m, 5H), 6.73-6.71(d, 2H), 4.60(s, 2H ), 4.17-4.15(d, 2H), 4.06-4.01(t, 2H), 3.81(s, 3H), 2.58-2.53(t, 2H);
[0103] ESI-MS(M / z): 517.6(M + +1)
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