CDI活化4-羟甲基苯硼酸频哪醇酯，求助
最近在做CDI(羰基二咪唑)，活化4-羟甲基频哪醇酯，得到活化酯，一开始按文献是可以制备得到固体产物的，可最近可能气温降低还是原材料变质，按原方法，萃取，无水硫酸钠吸水后，旋干乙酸乙酯后，始终无法得到固体，仅有一些液体状粘稠物，像凝胶，尝试延长反应时间，提高CDI比例仍无改善，不知有没有朋友做过类似反应，求教，十分感谢。
以下为文献方法：Compound S1 (7.37 g, 31.5 mmol) was dissolved in dry CH2Cl2 (46 mL) in a flame-dried 100-mL flask. Carbonyldiimidazole (10.20 g, 62.9 mmol) was added and the reaction was stirred for 30 min. The mixture was diluted in ethyl acetate (200 mL) and washed with H2O (3 x 10 mL). The organics were washed with brine (1 x 10 mL), dried over MgSO4, and concentrated in vacuo to give a pure white solid@celan@celan@celan@celan@yangtie2008
返回小木虫查看更多
今日热帖
京公网安备 11010802022153号
赡苁瞧碌停吹有Ч缓迷斐傻�
把粘稠膏状物置于饱和盐水中浸泡一晚上看看，
既然得到过产物，你把粘稠也对比一下就行了