反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
55.5 g (0.2 mol) of dimethyl N-butenoylaminoterephthalate are mixed with 175 mg of hexachloroplatinic acid (as a catalyst) and 85 g (0.8 mol; excess) of methyldimethoxysilane under an inert gas. Gas bubbles which form on the crystals of the catalyst indicate the immediate start of the reaction. The mixture is stirred up at short intervals of time, and after about half an hour is heated to the reflux temperature (about 60° C.) and kept under reflux for 25 hours. The reaction mixture is concentrated down to a deep-brown oil in vacuo. The oil is taken up in 400 ml of n-hexane, whereupon the product crystallizes out in the form of yellow crystals. 4-(Methyldimethoxysilyl)butanoic acid terephthalic acid dimethyl ester)amide is obtained by dissolving in hot n-hexane, crystallization in the cold and drying of the crystals in vacuo.
WORKUP
后处理
- customGas bubbles which form on the crystals of the catalyst
- customthe immediate start of the reaction
- temperatureunder reflux for 25 hours
- concentrationThe reaction mixture is concentrated down to a deep-brown oil in vacuo
- customcrystallizes out in the form of yellow crystals