A chiral aminomethyltriazole substituted tricyclic fluoroquinolone carboxylic acid derivative and its preparation method and application
A technology of fluoroquinolone carboxylic acid and aminomethyltriazole, which is applied in the field of innovative drug synthesis to achieve the effect of overcoming drug resistance
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Embodiment 1
[0044] S-(-)-9-fluoro-2,3-dihydro-3-methyl-10-(4-dimethylaminomethyl-[1,2,3]triazol-1-yl)-7- Oxo-7H-pyridine[1,2,3-de]-[1,4]benzoxazine-6-carboxylic acid (I-1), its chemical structure is:
[0045]
[0046] That is, R in formula I is dimethylamino.
[0047] The preparation method of the compound is as follows: using dimethylamine as the amine donor, according to the above-mentioned general preparation method of the target object (I), the light yellow crystal (I-1) is obtained, the yield is 66.0%, m.p.223-225°C . 1 H NMR (400MHz, DMSO-d 6 ): δ15.48(brs,1H,COOH),9.26(s,1H,5-H),7.87(s,1H,5″-H),7.72(d,J=13.2Hz,1H,8-H ),5.34(s,2H,NCH 2 ),4.94-4.56(m,3H,OCH 2 CH),2.47(s,6H,NCH 3 ), 1.47 (d, J=4.0Hz, CH 3 ); MS(m / z): Calcd.for C 18 h 18 FN 5 o 4 :387.37[M] + ;Found:388[M+H] + .
Embodiment 2
[0049] S-(-)-9-fluoro-2,3-dihydro-3-methyl-10-(4-diethylaminomethyl-[1,2,3]triazol-1-yl)-7- Oxo-7H-pyridine[1,2,3-de]-[1,4]benzoxazine-6-carboxylic acid (I-2), its chemical structure is:
[0050]
[0051] That is, R in formula I is diethylamino.
[0052] The preparation method of the compound is as follows: using diethylamine as the amine donor, according to the above-mentioned general preparation method of the target object (I), the light yellow crystal (I-2) is obtained, the yield is 53.0%, m.p.214-216°C . 1 H NMR (400MHz, DMSO-d 6 ):δ15.46(brs,1H,COOH),9.27(s,1H,5-H),7.86(s,1H,5″-H),7.74(d,J=13.2Hz,1H,8-H ),5.31(s,2H,NCH 2 ),4.93-4.52(m,3H,OCH 2 CH),2.45-2.34(m,4H,2×CH 2 ),1.48-1.17(m,6H,2×CH 3 ); MS(m / z): Calcd.for C 20 h 22 FN 5 o 4 :415.43[M] + ;Found:416[M+H] + .
Embodiment 3
[0054] S-(-)-9-fluoro-2,3-dihydro-3-methyl-10-(4-piperidin-1-methyl-[1,2,3]triazol-1-yl)- 7-oxo-7H-pyridine[1,2,3-de]-[1,4]benzoxazine-6-carboxylic acid (I-3), its chemical structure is:
[0055]
[0056] That is, R in formula I is piperidin-1-yl.
[0057] The preparation method of the compound is as follows: using piperidine as the amine donor, according to the above-mentioned general preparation method of the target object (I), the light yellow crystal (I-3) was obtained with a yield of 57.0%, m.p.224-226°C. 1 H NMR (400MHz, DMSO-d 6 ): δ15.43(brs,1H,COOH),9.25(s,1H,2-H),7.83(s,1H,5″-H),7.73(d,J=13.2Hz,1H,5-H ),5.28(s,2H,NCH 2 ),4.89-4.54(m,3H,OCH 2 CH),3.12-2.30(m,4H,N(CH 2 ) 2 ),1.62-1.15(m,9H,CH 3 and 3 x CH 2 ); MS(m / z): Calcd.for C 21 h 22 FN 5 o 4 :427.44[M] + ;Found:428[M+H] + .
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