A solution of R1 (4.5g, 8.9mmol) in DCE (50mL) was maintained at 0oC. And then R2 (6.4g, 44.5mmol) was added dropwise. After stirring at 0oC for 2 hours, the reaction mixture was warmed to reflux o/n. The mixture was evaporated under vacuum. The residue was added with MeOH(50mL)and then refluxed for 1 hour. The mixture was evaporated under vacuum and was added DCM 50mL and the saturated solution of NaHCO3(50mL). Then the organic layer was washed with the saturated solution of NaHCO3(50mL) 3 times a, dried over anhydrous Na2SO4 and then evaporated under vacuum to give the desired product ,
我刚做过脱苄基的反应,苄基连在酚氧基上,不知道对你的化合物是否合适
用TiCl,二氯甲烷作溶剂,室温,10分钟左右
效果很好
鈀碳脱苄基的同时把碳碳双键还原,可是结果把与C=C相邻的羰基给还原成羟基了,该怎么办啊?
Na和液氨还原可以除去bian基保留双键
这个反应我做过有段时间,当时碰到的是带有卤素的或者含有两个双建的化合物,用鈀碳脱苄基,结果是把双建给还原了,另外把卤素也给掉了。当然也用过甲酸胺之类的办法都解决不了,后来是使用“氯甲酸氯乙酯(R2)和甲醇”解决了。大致的操作步骤见下面(其中R1 为当时的底物):
A solution of R1 (4.5g, 8.9mmol) in DCE (50mL) was maintained at 0oC. And then R2 (6.4g, 44.5mmol) was added dropwise. After stirring at 0oC for 2 hours, the reaction mixture was warmed to reflux o/n. The mixture was evaporated under vacuum. The residue was added with MeOH(50mL)and then refluxed for 1 hour. The mixture was evaporated under vacuum and was added DCM 50mL and the saturated solution of NaHCO3(50mL). Then the organic layer was washed with the saturated solution of NaHCO3(50mL) 3 times a, dried over anhydrous Na2SO4 and then evaporated under vacuum to give the desired product ,
我做过黄酮化合物的脱苄基反应,结构中含有碳碳双键和羰基,常温常压下都没有掉的