Compounds and preparation method thereof, application of compounds in preparing antineoplastic drugs and antineoplastic drugs prepared from compounds
A technology of anti-tumor drugs and compounds, applied in the direction of anti-tumor drugs, steroids, drug combinations, etc., can solve the problems of low biological activity and selectivity, high toxicity, etc., and achieve high biological activity and selectivity, low toxicity, and stability good sex effect
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Embodiment 1
[0053] 4-(5-(1,3-Benzodioxane)-((3aR,4aS,8S,10aS,11S,12S,12aS)-(8,11,12-trihydroxy)-(10a,12a- Dimethyl)-(1,2-cyclopentyl)-1,10a-b-epoxy tetradecyl)-(4,5-dihydropyrazole))benzenesulfonamide (compound 46) preparation of
[0054]
[0055] Under stirring at -20°C, add the corresponding intermediate 34 (10.0 mmol) and dichloromethane (25 mL) obtained in step 5 to a 50 mL round-bottomed flask in sequence, and gradually add boron tribromide (5 mmol) dropwise to continue the reaction with stirring After 1 h, the reaction flask was transferred to room temperature, and the reaction was continued for 12 h. TLC tracking reaction (developing agent V AcOEt :V 正己烷 =1:2), after the reaction was completed, filtered, the solid was washed with distilled water, and finally dried in vacuo, and the obtained solid was dissolved in absolute ethanol for recrystallization and purification to obtain the crystalline target compound.
[0056] White crystals were obtained with a yield of 54.3%. m.p...
Embodiment 2
[0058] 4-(5-(4-methyl-1,3-benzodioxane)-((3aR,4aS,8S,10aS,11S,12S,12aS)-(8,11,12-trihydroxy)- (10a,12a-Dimethyl)-(1,2-cyclopentyl)-1,10a-b-epoxytetradecyl)-(4,5-dihydropyrazole))benzenesulfonate Preparation of Amide (Compound 47)
[0059]
[0060] The preparation method refers to Example 1. White crystals were obtained with a yield of 46.2%. m.p.219~220℃; 1 H NMR (DMSO-d 6 ,300MHz)δ:8.00(d,J=7.5Hz,2H,ArH),7.76(d,J=7.5Hz,2H,ArH),6.89(s,2H,NH 2 ), 5.91(d, J=4.7Hz, 1H, ArH), 5.82~5.67(m, 2H, ArH), 5.50(s, 1H, CH 2 ),5.40(dd,J 1 =11.3Hz,J 2 =11.1Hz,1H,CH 2 ), 5.39(s, 2H, OH), 4.48(s, 1H, OH), 4.15(d, J=10.1Hz, 1H, CH), 3.54~3.29(m, 5H, CH and CH 2 ),2.24~2.15(m,2H,CH 2 ), 2.01(t, J=4.5Hz, 1H, CH), 1.80~1.10(m, 18H, CH and CH 2 ),0.88(s,3H,CH 3 ),0.84(s,3H,CH 3 ).ESI-MS:682.9[M+H] + .Anal.Calcd for C 36 h 47 N 3 o 8 S: C, H, N.
Embodiment 3
[0062] 4-(5-(4,7-Dimethyl-1,3-benzodioxane)-((3aR,4aS,8S,10aS,11S,12S,12aS)-(8,11,12-tri Hydroxy)-(10a,12a-dimethyl)-(1,2-cyclopentyl)-1,10a-b-epoxytetradecyl)-(4,5-dihydropyrazole) ) Preparation of benzenesulfonamide (compound 48)
[0063]
[0064] The preparation method refers to Example 1. White crystals were obtained with a yield of 48.2%. m.p.199~200℃; 1 H NMR (DMSO-d 6 ,300MHz)δ:8.04(d,J=7.2Hz,2H,ArH),7.75(d,J=7.1Hz,2H,ArH),6.88(s,2H,NH 2 ), 5.92(d, J=4.7Hz, 1H, ArH), 5.80~5.67(m, 2H, ArH), 5.50(s, 1H, CH 2 ),5.40(dd,J 1 =11.2Hz,J 2 =11.4Hz,1H,CH 2 ), 5.37(s, 2H, OH), 4.49(s, 1H, OH), 4.12(d, J=9.5Hz, 1H, CH), 3.53~3.29(m, 5H, CH and CH 2 ),2.28~2.16(m,2H,CH 2 ), 2.01(t, J=4.2Hz, 1H, CH), 1.81~1.05(m, 20H, CH and CH 2 ),0.89(s,3H,CH 3 ),0.85(s,3H,CH 3 ).ESI-MS:696.9[M+H] + .Anal.Calcd for C 37 h 49 N 3 o 8 S: C, H, N.
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