HRID576458
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
1.5 g (37.5 mmol) of NaH (60% in oil) are initially introduced in 150 ml of dichloromethane. A solution of 8 g (28 mmol) of 12,12-dimethyl-6,12-dihydro-6-azaindeno[1,2-b]fluorene in dichloromethane is added dropwise at room temperature. After 1 h, 8.5 g (31 mmol) of 2-chloro-4,6-diphenyl-1,3,5-triazine are added dropwise, and the mixture is stirred at RT for 8 h. The solid which has precipitated out is recrystallised from toluene. The crystals which have deposited are filtered off with suction, washed with a little MeOH and dried in vacuo; yield: 11.6 g; 80% of theory; purity: 99.9% according to HPLC.
WORKUP
后处理
- customThe solid which has precipitated out
- customis recrystallised from toluene
- filtrationThe crystals which have deposited are filtered off with suction
- washwashed with a little MeOH
- customdried in vacuo