HRID1627746
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
6.3 g (22.2 mmol) of 8,8-dimethylindolo[3,2,1-de]acridine are initially introduced in 150 ml of CH2Cl2. A solution of 8 g (45.1 mmol) of NBS in 100 ml of acetonitrile is subsequently added dropwise at −15° C. with exclusion of light, and the mixture is allowed to come to room temperature and is stirred at this temperature for a further 4 h. 150 ml of water are subsequently added to the mixture, which is then extracted with CH2Cl2. The organic phase is dried over MgSO4, and the solvents are removed in vacuo. The product is washed by stirring with hot hexane and filtered off with suction. Yield: 4.5 g (12 mmol), 57% of theory, purity according to 1H-NMR about 97%.
WORKUP
后处理
- customto come to room temperature
- extractionis then extracted with CH2Cl2
- dry with materialThe organic phase is dried over MgSO4
- customthe solvents are removed in vacuo
- washThe product is washed
- stirringby stirring with hot hexane
- filtrationfiltered off with suction