Biguanide derivatives as dpp-iv inhibitors
A technology for preparing medicines and medicines, applied in anti-inflammatory agents, drug combinations, non-central analgesics, etc., can solve the problems of lack of hypoglycemia, weight, etc., achieve the effect of improving or restoring function and preventing β-cell degeneration
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[0056] The preparation of formula (III) compound
[0057] 1. Preparation of 8-bromo-7-(2-butyn-1-yl)-3-methyl-1-(quinolin-2-ylmethyl)-3,7-xanthine (compound III-1)
[0058]
[0059] (1) Preparation of 8-bromo-7-(2-cyanobenzyl)-1,3-dimethyl-3,7-xanthine
[0060] Mix 3-methyl-8-bromo-xanthine with N-ethyldiisopropylamine (DIPEA) in N,N-dimethylformamide, add 2-cyanobenzyl bromide, and Stir overnight. For work-up, the reaction mixture was poured into water. The separated precipitate is suction filtered, washed with water, and dried to obtain 3-methyl-7-(2-cyanobenzyl)-8-bromo-xanthine (molecular formula: C 14 h 10 BrN 5 o 2 ).
[0061] Mass spectrometry (ESI + ): m / z=36[1M+H] + ;
[0062] Elemental analysis: C, 46.69; H, 2.80; Br, 22.19; N, 19.44; O, 8.88.
[0063] (2) Preparation of 8-bromo-7-(2-cyanobenzyl)-3-methyl-1-(quinolin-2-ylmethyl)-3,7-xanthine
[0064] Add 2-bromomethylquinoline to a mixed solution of 3-methyl-7-(2-cyanobenzyl)-8-chloro-xanthine an...
Embodiment 1
[0118] Example 1: l-(quinolin-2-ylmethyl)-3-methyl-7-(2-cyanobenzyl)-8-((R)-3-(N1-n-butylbiguanide base )-piperidin-1-yl)-xanthine (compound I-1) preparation
[0119]
[0120] Dissolve dicyandiamide in isopropanol, add (R)-8-(3-n-butylaminopiperidin-1-yl)-7-(2-cyanobenzyl)-3-methyl-1 -(quinolin-2-ylmethyl)-3,7-xanthine (compound II-1), adjust the pH to 5-6 with 36% HCl, control the temperature at 80-100°C for 6 hours, let stand after the reaction is completed After cooling, a large amount of white crystals were precipitated, filtered by suction, washed, dried and recrystallized with absolute ethanol to obtain the title compound (molecular formula: C 35 h 40 N 12 o 2 ).
[0121] Mass spectrometry (ESI + ): m / z=661[M+H] +
[0122] Elemental analysis: C, 63.62; H, 6.10; N, 25.44; O, 4.84.
[0123] 1 H-NMR (d6-DMSO): 8.06(1H), 8.01(1H), 7.83(2H), 7.75(1H), 7.63(1H), 7.52(3H), 7.46(1H), 7.30(2H), 6.62 (2H), 5.47(2H), 4.76(2H), 3.61(1H), 3.39(3H), 3.34(1H), 3.30(2H), 3...
Embodiment 2
[0124] Example 2: l-benzyl-3-methyl-7-(2-cyanobenzyl)-8-((R)-3-(N1-n-butylbiguanidinyl)-piperidin-1-yl )-xanthine (compound 1-2) preparation
[0125]
[0126] Dissolve dicyandiamide in isopropanol, add (R)-8-(3-n-butylaminopiperidin-1-yl)-7-(2-cyanobenzyl)-3-methyl-1 -Benzyl-3,7-xanthine (compound II-2), adjust the pH to 5-6 with 36% HCl, control the temperature at 80-100°C for 6.5 hours, leave it to cool after the completion of the reaction, a large amount of white crystals precipitated, pumped Filter, wash, recrystallize with absolute ethanol after drying, obtain title compound (molecular formula: C 32 h 39 N 11 o 2 ).
[0127] Mass spectrometry (ESI + ): m / z=610[M+H] +
[0128] Elemental analysis: C, 63.04; H, 6.45; N, 25.27; O, 5.25.
[0129] 1 H-NMR (d6-DMSO): 7.84(2H), 7.55(3H), 7.20-7.53(6H), 6.63(2H), 5.46(2H), 5.01(2H), 3.60(1H), 3.35(1H) , 3.38(3H), 3.34(2H), 3.27(2H), 2.63(1H), 2.15(1H), 1.83(1H), 1.48-1.58(5H), 1.30(2H), 0.89(3H).
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