将DON(79.0mg,0.27mmol)溶解在50mL无水二氯甲烷中,加入吡啶(1 mL)和4-DMAP(约10 mg),然后逐滴加入乙酸酐(27.2 mg,0.27mmol).将反应搅拌过夜,用20mL HCl(2N)处理,并用50毫升二氯甲烷萃取3次.用硫酸钠干燥后,过滤并蒸发溶剂.剩余的残余物进行柱色谱分离(CHCl 3 :MeOH = 95:5),得到15-ADON即15-O-乙酰脱氧瓜萎镰菌醇(42.0 mg,47%,). 1 H NMR(200 MHz,CDCl 3)δ= 6.61(dq,J = 5.7,1.6 Hz,1H),4.89(d,J = 5.7 Hz,1H),4.83(d,J = 1.6 Hz,1H),4.52(dt,J = 10.2,4.7 Hz,1H),4.24(s,2H),3.78(d,J = 1.8 Hz,1H),3.63(d,J = 4.5 Hz,1H),3.13(d,J = 4.3 Hz,1H),3.08(d,J = 4.3 Hz),1H),2.22(dd,J = 14.8,4.7 Hz,1H),2.08(dd,J = 14.7,10.4 Hz,1H),1.88(s,3 H),1.87(s,3H),1.07(s,3H); 13 C-NMR(50 MHz,CDCl 3)δ= 199.6(s),170.3(s),138.8(d),135.6(s),80.7(d),73.5(d),70.1(d),68.9(s),65.5(s),62.2(t),51.4(s),47.4(t),46.3(s),43.3(t),20.7(q),15.4(q),13.8(q).
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