化学合成。
化学合成
合成路线 1(1. 合成:2491-18-1)
产率:98%
合成条件:at 0℃; for 16 h; Inert atmosphere; Reflux
实验步骤:合成实施例1将L-甲硫氨酸(0.5g,1当量)悬浮在装有磁力搅拌器的100ml烧瓶中的甲醇(30ml C = 0.1M)中并置于氮气下。 在0℃下将亚硫酰氯(0.5ml,2当量)滴加到该溶液中,然后在回流下加热16小时。 然后蒸发反应混合物,得到浅黄色固体。 将固体用热乙醚研磨,弃去溶液,得到标题化合物2,为白色固体,将其进一步真空干燥。 (0.65561g,98%收率).1 H NMR(D20,500MHz)δH:4.24(1H,m,3)3.79(3H,s,1),2.63(2H,t,5),2.25(1H,m) ,4),2.16(1H,m,4),2.06(1H,s,6)13C NMR(D20,125MHz)6C:170.58(2),53.64(1),51.70(3),28.71(4), 28.41(5),13.85(6).IR(neat,vmax,cnV1):2880.8 / 2676,2(CH3,CH2,CH),2016.2,1742.2(C = 0,酯),1483.6,1443.5,1227 + 1194.7 + 1149.8 + 1079.5(CO).HRMS m / z(+ ESI):C 6 H 14 NO 2 S,质量分析= 64.074(误差= 0.07ppm)
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