化学合成。
化学合成
合成路线 1(1. 合成:6089-04-9)
产率:97.2%
合成条件:With toluene-4-sulfonic acid In dichloromethane at 0 - 20℃; for 1 h;
实验步骤:O-THP炔丙醇(18)化合物18根据文献程序制备.24至炔丙醇17(2.6mL,44.6mmol)和p-TsOH一水合物(0.09g,0.5mmol)在CH 2 Cl 2(45mL)中的溶液在0℃下滴加DHP(4.3mL,46.8mmol)。在0℃下搅拌5分钟后,将反应混合物温热至室温并搅拌1小时。接下来,将反应混合物用饱和NaHCO 3(30mL)洗涤,并将水层用CH 2 Cl 2(45mL)萃取。合并的有机层经MgSO 4干燥,过滤,并在减压下浓缩,得到化合物18(6.1g,97.2%),为黄色油状物。 Rf = 0.30(正己烷/ Et2O 95/5)。 1H NMR(400MHz,CDCl3):δ= 1.50-1.67(m,4H),1.70-1.89(m,2H),2.41(t,J = 2.4Hz,1H),3.52-3.57(m,1H),3.82 -3.87(m,1H),4.27(ddd,J = 2.4Hz,11.3Hz,15.8Hz,2H),4.83(t,J = 3.4Hz,1H)。 13 C NMR(100MHz,CDCl 3):δ= 19.0,25.3,30.2,53.9,61.9,74.0,79.7,96.8。 MS-CI:m / z计算值C 8 H 12 O 2 [M + H] +,141;实测值:141。发现,141。此化合物也曾在此前报道过
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