Dabigatran derivatives
A technology of dabigatran and its derivatives, which is applied in the field of dabigatran derivatives and can solve the problems of further improvement of oral bioavailability
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Embodiment 1
[0080] Example 1N-{[2-(((4-N-hexyloxycarbonyl-amidino-phenyl)-amino)-methyl)-1-methyl-1H-benzimidazol-5-yl]-carbonyl Preparation of}-N-(pyridin-2-yl)-β-alanine (9)
[0081] Dissolve 9 g of dabigatran etexilate with 250 ml of methanol, stir at room temperature, add 80 ml of an aqueous solution containing 3.6 g of LiOH, and stir for 60 minutes. Add 150ml of water, neutralize with 1N dilute hydrochloric acid, and a solid precipitates out. Filter and dry the solid to obtain 97.4 g of the target compound. 1 H NMR δ (ppm, DMSO-d 6 ): 0.89(t, 3H), 1.31(m, 6H), 1.60(m, 2H), 2.71(t, 2H), 3.79(s, 3H), 3.98(t, 2H), 4.25(t, 2H) , 4.62(d, 2H), 6.75(d, 2H), 6.90(d, 1H), 6.97(t, 1H), 7.14(m, 2H), 7.41(d, 1H), 7.49(d, 1H), 7.56 (m, 1H), 7.82 (d, 2H), 8.41 (m, 1H), 8.50-9.30 (bs, 2H), 12.15 (s, 1H).
Embodiment 2
[0082] Example 2N-{[2-(((4-N-hexyloxycarbonyl-amidino-phenyl)-amino)-methyl)-1-methyl-1H-benzimidazol-5-yl]-carbonyl }-N-(pyridin-2-yl)-β-alanine acetoxymethyl ester (I 1 ) preparation
[0083]
[0084] Dissolve 0.4 g of intermediate 9 in 8 ml of DMF, blow dry nitrogen, stir at room temperature, and add 0.3 ml of triethylamine. With stirring, 0.1 ml of chloromethyl acetate was added dropwise. After the addition, the temperature was gradually raised to 50° C., and the reaction was stirred for 5 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in 50 ml of ethyl acetate and washed with water; the organic layer was dried over anhydrous sodium sulfate overnight. Filter, evaporate the organic solvent under reduced pressure, separate the residue by silica gel column chromatography, elute with dichloromethane:methanol (30:1) mixed solvent, collect the required components, and evaporate to dryness under reduced pressure to obtain the target co...
Embodiment 3
[0085] Example 3N-{[2-(((4-N-hexyloxycarbonyl-amidino-phenyl)-amino)-methyl)-1-methyl-1H-benzimidazol-5-yl]-carbonyl }-N-(pyridin-2-yl)-β-alanine isobutyryloxymethyl ester (I 4 ) preparation
[0086]
[0087] With reference to the method of Example 2, 0.4g of intermediate 9 was reacted with chloromethyl isobutyrate and separated by silica gel column chromatography to obtain the target compound I 4 0.28g. 1 H NMR δ (ppm, DMSO-d 6 ): 0.89(t, 3H), 1.14(d, 6H), 1.31(m, 6H), 1.60(m, 2H), 2.53(m, 1H), 2.71(t, 2H), 3.79(s, 3H) , 3.98(t, 2H), 4.25(t, 2H), 4.62(d, 2H), 5.61(s, 2H), 6.75(d, 2H), 6.90(d, 1H), 6.97(t, 1H), 7.14(m, 2H), 7.41(d, 1H), 7.49(d, 1H), 7.56(m, 1H), 7.82(d, 2H), 8.41(m, 1H), 8.50-9.30(bs, 2H) .
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