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
18.80 g of 1-{6-[1-(2-chloro-4,6-dimethylphenylimino)-ethyl]pyridin-2-yl}ethanone (0.0625 mol), 22.16 g of 2,6-diisopropylaniline (0.125 mol) and 20.0 g of Sicapent were heated under reflux under argon in 300 ml of tetrahydrofuran for 17 h. A further portion of Sicapent (10.0 g) was added and the mixture was heated under argon for a further 4 h and then cooled to room temperature. It was filtered and the residue on the filter was washed with 50 ml of tetrahydrofuran. The solvent was distilled off completely from the combined filtrates and the residue was stirred with 50 ml of methanol. The precipitate formed was filtered off, washed twice with methanol, stirred with 100 ml of hot methanol and then filtered. 17.84 g (0.0388 mol) of 2-[1-(2-chloro-4,6-dimethylphenylimino)ethyl]-6-[1-(2,6-diisopropylphenylimino)ethyl]pyridine were obtained in a yield of 62%.
WORKUP
后处理
- additionA further portion of Sicapent (10.0 g) was added
- temperaturethe mixture was heated under argon for a further 4 h
- filtrationIt was filtered
- washthe residue on the filter was washed with 50 ml of tetrahydrofuran
- distillationThe solvent was distilled off completely from the combined filtrates
- customThe precipitate formed
- filtrationwas filtered off
- washwashed twice with methanol
- stirringstirred with 100 ml of hot methanol
- filtrationfiltered