2,6-二溴-4-甲基吡啶

2,6-二溴-4-甲基吡啶制备... ' style="background-color:rgba(0,0,0,0)!important;border-bottom-color:rgb(51,51,51);border-style:none;border-image-repeat:stretch;border-image-slice:100%;border-image-source:none;color:rgb(51,51,51);font-size:13px;font-style:normal;font-variant:normal;font-weight:400;letter-spacing:normal;list-style:outside none none;margin:0px;orphans:2;padding:0px;text-align:left;text-decoration:none;text-indent:0px;text-transform:none;vertical-align:middle;word-spacing:0px;background-blend-mode:normal!important;background-clip:content-box!important;background-position:50% 50%!important;background-image:var(--sf-img-6)!important;background-size:100% 100%!important;background-origin:content-box!important;background-repeat:no-repeat!important">
具体步骤...将θ-羟基^-甲基^-氧代^^-二氢-S-吡啶甲腈盐酸盐(D1,5g,30.94mmol)和氧溴化磷(25g,87.2mmol)在13℃一起加热6小时.将混合物在冰中冷却,并小心地添加水,然后将混合物用2M氢氧化钠溶液碱化并用二氯甲烷萃取.分离有机相并蒸发,得到浅棕色固体.将其通过硅胶色谱法(CombiFlashCompanion,Redisep80g硅胶柱)纯化,用环己烷-二氯甲烷混合物(100%-70%环己烷)洗脱.合并包含主要成分的级分并蒸发,得到标题化合物(1.279g,16%),为无色固体.LCMS(方法A):单峰,Rt＝3.09mins;m/z.MH+250,252,254.
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