Pyrimido 1,2,4-triazole compound and its preparation method and application
A – technology of triazoles, compounds, applied in the field of medicinal chemistry
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Embodiment 1
[0075] This embodiment provides a compound e1, the structural formula of the compound e1 is as follows:
[0076]
[0077] The preparation method of the compound e1 comprises the following steps:
[0078] (1) Preparation of Compound M Add 1g (about 8.61mmoL) of 2-amino-5-mercapto-1,2,4-triazole and 1.37g (about 12.92mmoL) of sodium carbonate into the reaction flask respectively, and then About 20 mL of acetone was added, 1.13 mL (about 9.47 mmoL) of benzyl chloride was slowly added dropwise, and the reaction was refluxed at 60° C., and the reaction was monitored by TLC. After the reaction was completed, suction filtration was performed directly, and the filtrate was subjected to column chromatography (dichloromethane:methanol=20:1) to obtain pure compound M. Calculation by measurement: the yield of compound M is about 67.57%. Appearance: white solid. 1 H NMR (400MHz, DMSO-d 6 )δ7.41-7.18(m,5H),4.34(s,2H); 13 CNMR (100MHz, DMSO-d 6 )δ152.19, 147.08, 136.55, 128.79, 128....
Embodiment 2
[0083] This embodiment provides a kind of compound e2, and the structural formula of this compound e2 is as follows:
[0084]
[0085] This embodiment provides the preparation method of the above-mentioned compound e2, which is basically the same as the preparation method of the compound e1 provided in Example 1.
[0086] The compound e2 is a white solid with a calculated yield of about 90.1% and a melting point of 201.4°C-203.7°C; 1 H NMR (400MHz, DMSO-d 6 )δ11.22(s,1H),6.82(s,1H),5.00(t,J=6.2Hz,2H),3.71(s,2H),3.21(t,J=7.1Hz,2H),2.81( s,6H),1.85–1.69(m,2H),1.02(t,J=7.3Hz,3H); 13 C NMR (100MHz, DMSO-d 6 )δ166.73, 164.35, 154.60, 146.05, 141.80, 108.38, 54.07, 43.09, 42.42, 32.52, 24.53, 22.49, 13.04; HRMS (ESI): m / z calcdfor C 14 h 22 N 9 S 2 (M+H) + , 380.14341; found, 380.14078; therefore, it can be determined that the structural formula of the compound e2 provided in this example is as shown above.
Embodiment 3
[0088] This embodiment provides a compound e3, the structural formula of the compound e3 is as follows:
[0089]
[0090] This embodiment provides the preparation method of the above-mentioned compound e3, which is basically the same as the preparation method of the compound e1 provided in Example 1.
[0091] The compound e3 is a white solid with a calculated yield of about 93.3% and a melting point of 174.2°C-175.8°C; 1 H NMR (400MHz, DMSO-d 6 )δ11.15(s,1H),6.82(s,1H),6.02(m,1H),5.38(d,J=17.0Hz,1H),5.16(d,J=10.0Hz,1H),5.00( t, J=6.2Hz, 2H), 3.92(d, J=6.8Hz, 2H), 3.70(s, 2H), 2.81(s, 6H); 13 C NMR (100MHz, DMSO-d 6 )δ166.01, 164.50, 154.59, 146.01, 141.98, 133.38, 118.50, 108.44, 54.07, 43.09, 42.41, 33.20, 24.55; HRMS (ESI): m / z calcd for C 14 h 20 N 9 S 2 (M+H) + , 378.12776; found, 378.12473; therefore, it can be determined that the structural formula of the compound e3 provided in this example is as shown above.
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