化学合成。
医药合成
合成路线 1(1. 合成:74597-04-9)
产率:86.3%
合成条件:With phosphorus tribromide In dichloromethane at 0 - 20℃; for 1 h;
实验步骤:中间体17:3-(溴甲基)苯酚向装有磁力搅拌器的50mL RB烧瓶中加入15mL二氯甲烷。 向搅拌的溶剂中加入3-羟甲基 - 苯酚(0.5g,4.03mmol)。 将RM调至0并逐滴加入亚磷酸三钠(1.6g,0.56mL,6.04mmol)。 添加后,将RM在室温下搅拌1小时。 1小时后,将RM用二氯甲烷(25mL)稀释,并将有机层用水(20mL)洗涤。 将有机层用无水Na 2 SO 4干燥,减压除去溶剂。 得到棕色固体产物。 (0.65g,收率:86.3%); MS(ESI,120eV):m / z = 187.0(M + H)+。 1H NMR(300MHz,CDCl3):δ7.10-7.15(t,1H),6.86-6.89(d,1H),6.80(d,1H),6.67-6.71(m,1H),4.35-4.36 (d,2H),3.80-3.94(bro s,1H)。
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