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
PROCEDURE
实验过程
To a solution of 2.45 g (8.80 mmol) of 2,7-di-tert-butylfluorene in 50 ml of THF, 5.67 ml (9.24 mmol) of a hexane solution of n-butyllithium was dropwise added in a nitrogen atmosphere at 0° C., followed by stirring at room temperature overnight. To the resulting solution, a solution of 2.85 g (17.6 mmol) of 3-tert-butyl-6,6-dimethylfulvene in 30 ml of THF was successively dropwise added in a nitrogen atmosphere at 0° C., followed by stirring at room temperature overnight to perform reaction. After the reaction, 30 ml of water was added. The organic phase was extracted with ether and dried over anhydrous magnesium sulfate. From the resulting solution, the solvent was distilled off to obtain a crude yellow solid. The solid was washed with methanol to obtain 2.77 g of a powdery white solid (yield: 71.5%). The analyzed values are given below.
WORKUP
后处理
- stirringby stirring at room temperature overnight
- customreaction
- additionwas added
- extractionThe organic phase was extracted with ether
- dry with materialdried over anhydrous magnesium sulfate
- distillationFrom the resulting solution, the solvent was distilled off
- customto obtain a crude yellow solid
- washThe solid was washed with methanol