Pyrimidine thioacetamide derivatives, preparation method and application thereof
A technology of pyrimidine thioacetamide and its derivatives, applied in the field of medicine, can solve problems such as the spread of drug-resistant strains and the threat of clinical application, and achieve the effect of great development value
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Embodiment 1
[0041] Embodiment 1: Preparation of N-(4-sulfonamido-2-bromophenyl)-2-(5-(naphthalene-1-yl)pyrimidin-4-ylmercapto)acetamide (Ia-1)
[0042] 5-Bromo-4-hydroxypyrimidine (IIa) (0.10g, 0.57mmol), 1-naphthaleneboronic acid (IIIa) (0.12g, 0.69mmol), tetrakistriphenylphosphine palladium (0.066g, 0.057mmol), sodium carbonate (0.18g, 1.7mmol) were weighed in a 50mL round-bottomed flask, and a mixed solvent of dioxane and water (5:1, 12mL) was added, replaced with nitrogen three times, and heated to 90°C in an oil bath for 6 hours. The reaction solution was cooled to room temperature, dioxane was distilled off under reduced pressure, 20 mL of water was added, extracted with ethyl acetate (2×10 mL), the organic layers were combined, washed with sodium hydroxide water (1mol / L, 2×10 mL), combined with water The pH of the layer was adjusted to 3 with dilute hydrochloric acid, and a large amount of white solid precipitated out, which was filtered and dried to obtain intermediate IVa. White...
Embodiment 2
[0045] Embodiment 2: Preparation of 3-bromo-4 (2-(5-naphthalene-1 base) pyrimidin-4-yl mercapto) acetamide) methyl benzoate (Ia-2)
[0046] The operation method is the same as the preparation of Example 1 (Ia-1), except that methyl 3-bromo-4-(2-chloroacetamido)benzoate is used. White powder, yield: 56.3%.mp:148-151℃. 1 HNMR (400MHz, DMSO-d 6 ,ppm)δ:9.36(s,1H,NH),9.17(s,1H,pyrimidine-H),8.47(d,1H,J=5.56Hz,PhH),8.45(s,1H,pyrimidine-H), 8.21(d,1H,J=1.92Hz,PhH),8.01-7.94(m,3H,naphthalene-H,PhH),7.59-7.53(m,2H,naphthalene-H),7.46-7.43(m,3H, naphthalene-H), 4.05(d, J=15.0Hz, 1H, CH 2 ),3.92-3.88(m,4H,CH 2 ,CH 3 ). 13 C-NMR (100MHz, DMSO-d 6 , ppm) δ: 167.79 (C=O), 167.16 (C=O), 165.34 (C 6 -pyrimidine), 157.52 (C 2 -pyrimidine), 155.33 (C 3 -pyrimidine), 139.80, 133.78, 132.24, 131.08, 130.54, 130.17, 129.87, 128.78, 128.08, 127.11 (2×C), 126.75, 126.62, 125.37, 124.62, 120.99, 112.312 (O 3 ),34.33(S-CH 2 ).ESI-MS: m / z508.3(M+1),510.3(M+3),512.7(M+5),530.2(M+23),C 24 h ...
Embodiment 3
[0047] Embodiment 3: Preparation of ethyl 3-bromo-4 (2-(5-naphthalene-1 base) pyrimidin-4-yl mercapto) acetamide) benzoate (Ia-3)
[0048] The operation method is the same as the preparation of Example 1 (Ia-1), except that ethyl 3-bromo-4-(2-chloroacetamido)benzoate is used. White powder, yield: 59.2%.mp:130-132℃. 1 HNMR (400MHz, DMSO-d 6 ,ppm)δ:9.32(s,1H,NH),9.18(s,1H,pyrimidine-H),8.46(s,1H,PhH),8.44(s,1H,pyrimidine-H),8.21(d,1H ,J=1.88Hz,PhH),8.01-7.94(m,3H,naphthalene-H,PhH),7.60-7.53(m,2H,naphthalene-H),7.48-7.42(m,3H,naphthalene-H), 4.39(q, 2H, J=7.12Hz, CH 2 ),4.06(dd,2H,J 1 =53.08Hz,J 2 =15.00Hz,CH 2 ),1.40(t,3H,J=7.12Hz,CH 3 ). 13 C-NMR (100MHz, DMSO-d 6 , ppm) δ: 168.32 (C=O), 167.01 (C=O), 164.85 (C 6 -pyrimidine), 157.16 (C 2 -pyrimidine), 154.81 (C 3 -pyrimidine), 139.64, 133.77, 133.71, 132.30, 131.04, 130.38, 130.24, 129.85, 128.80, 128.09, 127.15 (2×C), 126.65, 125.38, 124.58, 120.96, 112.290, 6 3 ),34.40(S-CH 2 ), 14.31 (CH 3 ).ESI-MS: m / z522.3...
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