Pyrimidine-type antitumor compound, preparation method and application thereof
A compound and anti-tumor technology, applied in the field of medicine, can solve problems such as reducing bioavailability
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Embodiment 1
[0089] Preparation of N'-phenyl-3-(uracil-5-sulfonamido)benzohydrazide (A1).
[0090] a. Preparation of uracil-5-sulfonyl chloride: Add uracil (6g, 53.55mmoL) and thionyl chloride (10mL, 89.22mmoL) into a 100mL reaction flask at 25°C, react at room temperature for 1.5h, add Chlorosulfonic acid (16g, 133.82mmoL) was reacted at 60°C for 4h, and continued to react at 75°C for 7h; the reaction solution was added to ice water, and a precipitate was precipitated, filtered with suction, washed with water several times, and dried at 50°C to obtain 4.50g of a white solid, yield : 70%.
[0091] b. Preparation of N'-(3-formic acid phenyl)uracil-5-sulfonamide: Add uracil-5-sulfonyl chloride (4g, 19.05mmol) in 20ml reaction bottle at 25°C In DMF, react with m-aminobenzoic acid (3.0 g, 22.86 mmol) in pyridine (0.6 g, 28.57 mmol) at room temperature for 5 h to obtain 5.00 g of the target product with a yield of 79.96%.
[0092] c. Preparation of N'-phenyl-3-(uracil-5-carboxamido)benzohydra...
Embodiment 2
[0095] Preparation of N'-(2-methylphenyl)-3-(uracil-5-sulfonamido)benzohydrazide (A2).
[0096] Using o-methylphenylhydrazine hydrochloride as raw material, synthesize uracil-5-sulfonyl chloride according to the steps of Example 1a, and prepare N'-(2-methylphenyl)-3-(urine Pyrimidine-5-sulfonamido)benzohydrazide, light yellow solid 2.08g, yield: 62.34%.
[0097] 1 H NMR (600MHz, DMSO-d 6)δ11.84(s.,1H),11.59(s.,1H),10.36(d,J=2.8Hz,2H),8.10(s,1H),7.62(d,J=2.1Hz,2H), 7.40(t, J=8.1Hz, 1H), 7.30(dd, J=1.1, 8.1Hz, 1H), 7.26(d, J=2.6Hz, 1H), 7.09-6.98(m, 2H), 6.72-6.62 (m,2H),2.20(s,3H); MS(ESI,m / z):414.08[M-H] - .
Embodiment 3
[0099] Preparation of N'-(3-methylphenyl)-3-(uracil-5-sulfonamido)benzohydrazide (A3).
[0100] Using m-methylphenylhydrazine as a raw material, synthesize uracil-5-sulfonyl chloride according to the step 1a of Example 1a, and prepare N'-(3-methylphenyl)-2-(uracil -5-sulfonamido)benzohydrazide (A3) off-white solid 2.58g, yield: 77.33%.
[0101] 1 H NMR (600MHz, DMSO-d 6 )δ10.47(s,1H),10.41(s,1H),8.11(s,1H),7.74(s,1H),7.71(d,J=5.8Hz,1H),7.64(s,1H), 7.59(d, J=7.7Hz, 1H), 7.41-7.40(m, 2H), 7.39(s, 1H), 7.32(d, J=7.3Hz, 1H), 2.38(s, 3H); MS(ESI ,m / z):414.10[M-H] - .
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