A 7-position chalcone derivative of benzoborazole and its preparation and application
A technology of chalcone derivatives and benzoborazole, which is applied in the field of chalcone derivatives at the 7-position of benzoborazole and its preparation and application, can solve the problems of less research in the field of anti-tumor, and achieve simple and efficient synthesis. Low cost, good suppression effect
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Embodiment 1
[0025] (E)-1-phenyl-3-(1-hydroxy-1,3-dihydro-benzo[c][1,2]borazol-7-yl)-2-propenone (1)
[0026]
[0027] Acetophenone (223 mg, 1.85 mmol) and sodium hydroxide (245 mg, 6.15 mmol) were added to a mixed solvent of ethanol (8 mL) and water (2 mL). After stirring at room temperature for 10 minutes, compound 1-hydroxy-7-formyl-1,3-dihydro-benzo[c][1,2]borazole (200 mg, 1.23 mmol) was added and stirred overnight at room temperature. The pH value of the reaction solution was adjusted to 3 with 1M hydrochloric acid and then filtered. The filter cake was purified by silica gel column chromatography (dichloromethane / methanol=250 / 1), and the obtained product was further slurried with n-hexane / ethyl acetate=3 / 1 to obtain compound 1 (90.0 mg, 27.6%). 1 H NMR (400MHz, DMSO-d 6 ): δ9.38(s,1H),8.22(d,J=16.0Hz,1H),8.15(d,J=7.8Hz,2H),8.10(d,J=16.0Hz,1H),8.04(d ,J=7.6Hz,1H),7.69(t,J=7.6Hz,1H),7.58(t,J=7.8Hz,3H).7.47(d,J=7.6Hz,1H),5.04(s,2H ) ppm; 13 C NMR (100MHz, DMSO-d 6 ):δ189.4,154...
Embodiment 2
[0029] (E)-1-(naphthalen-1-yl)-3-(1-hydroxy-1,3-dihydro-benzo[c][1,2]borazol-7-yl)-2-propenone (2)
[0030]
[0031] Synthetic method is similar to embodiment 1, and difference is:
[0032] (1) Soluble in an aqueous solution of methanol, wherein the volume ratio of methanol to water is 0.5:1;
[0033] (2) NaOH:
[0034] (3) The reaction time was 72 hours. After the reaction, the pH was adjusted to 1 with hydrochloric acid, and the compound 2 (72.5 mg, 62.3%) was finally obtained by beating. 1 H NMR (400MHz, DMSO-d 6 ):δ9.23(s,1H),8.36-8.34(m,1H),8.16(d,J=8.2Hz,1H),8.12(d,J=16.0Hz,1H),8.06-8.03(m, 1H), 8.01(dd, J=7.2, 1.0Hz, 1H), 7.96(d, J=7.6Hz, 1H), 7.75(d, J=16.0Hz, 1H), 7.67-7.60(m, 3H), 7.56(t, J=7.6Hz, 1H), 7.47(d, J=7.6Hz, 1H), 5.03(s, 2H)ppm; 13 C NMR (100MHz, DMSO-d 6 ):δ154.6,143.6,137.6,136.2,133.3,131.7,131.1,129.8,128.4,127.8,127.5,127.4,126.3,125.3,125.1,124.7,123.2,69.6ppm; HRMS(ESI):[M+H] + C 20 h 16 BO 3 calcd 315.1192, found 315.1196; mp: 1...
Embodiment 3
[0036] (E)-1-(furan-2-yl)-3-(1-hydroxy-1,3-dihydro-benzo[c][1,2]borazol-7-yl)-2-propenone (3)
[0037]
[0038] Synthetic method is similar to embodiment 1, and difference is:
[0039] (1) Soluble in an aqueous solution of methanol, wherein the volume ratio of ethanol to water is 10:1;
[0040] (2) NaOH:
[0041] (3) The reaction time was 0.5 h. After the reaction, the pH was adjusted to 6.9 with hydrochloric acid, and the compound 3 (43.0 mg, 45.7%) was finally obtained by beating. 1H NMR (400MHz, DMSO-d 6 ): δ9.36(s, 1H), 8.21(d, J=16.0Hz, 1H), 8.07(d, J=1.6Hz, 1H), 8.01(d, J=7.6Hz, 1H), 7.86(d ,J=16.0Hz,1H),7.78(d,J=3.6Hz,1H),7.57(t,J=7.6Hz,1H),7.47(d,J=7.6Hz,1H),6.80(dd,J =3.6,1.6Hz,1H),5.04(s,2H)ppm; 13 CNMR (100MHz, DMSO-d 6 ):δ176.8,154.5,152.9,148.2,141.3,137.6,131.0,125.1,123.0,122.9,119.2,112.5,69.6ppm; HRMS(ESI):[M+H] + C 14 h 12 BO 4 calcd 255.0829, found 255.0833; mp: 126-129°C; HPLC: purity 99.3%, retention time 15.3min.
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