二甲基铜锂烷基化反应求助?做一个反应(见附件),按照文献的方法(一模一样),之前可以做成功,最近 重复 了好多次,却怎么也得不到产物,更换了各种 试剂 都不行,各位大侠有没有经验指点非常感谢 (2S.3Rl-EthyI 2-Methyl-3-(tosylamino)pentanonfe (12). To a suspension of CuI (2.33 g, 12.2. mmol) in dry THF (25 ml), stirred at -78" under N2, was added 1 . 5 ~M eLi in Et,O (15.27 ml, 22.9 mmol). The resulting suspension was briefly warmed to 0" to dissolve solids and then recooled to -78". Next, the flask was immersed in an EtOH bath at -30", and a soh. of crude 11 (1.074 g, 2.53 mmol) in dry THF (25 ml) was added to the clear brown soln. The soln. was stirred at -2OO for 5 h at which time sat. aq. NH4CI soh. was added cautiously. After warming to r.t., H,O (40 ml) was added, the mixture acidified, then neutralized with aq. NaHCO, soln., filtered by suction, and extracted with AcOEt (4 x 15 ml). The combined org. phase was dried (Na2S04) and evaporated and the crude oil (0.917 g) purified by FC (31 x 2 cm, hexane/AcOEt 1:l): QQ图片20190306214612.png查看更多3个回答 . 4人已关注
乙二胺凝固成固体了,如何才能变成液体呢?冬天,实验室温度低,乙二胺凝固成固体了,现在打算用乙二胺溶剂热反应,如何才能变成固体呢? 我在百度上查了,乙二胺储存注意事项:储存于阴凉、通风的库房。远离火种、热源。库温不宜超过30℃。 求助各位虫虫,有什么办法可以变成液体了 b7e1d9e671253b3862169e0e4a84bac.jpg d7f6cc162b05373c7acdcf3a1364330.jpg [ last edited by wu1309122143 on 2019-3-1 at 20:44 ]查看更多4个回答 . 20人已关注