反应详情

A mixture of sodium hydride (0.48 g; 0.01 mol as 50% dispersion in oil) and THF (25 ml) is prepared and maintained under a nitrogen atmosphere. Then 3-[3-chloro-4-(phenethyloxy)phenyl]-1,1-dimethylurea (3.19 g; 0.01 mol) is added to the above mixture. Hydrogen is evolved and a thick paste forms. After about 15 minutes methyl iodide (1.4 g; 0.01 mol) is added and the reaction mixture stirred for two hours at room temperature. After two hours reaction time the paste redissolves. Next, most of the THF is removed under vacuum, the residue dissolved in methylene chloride. The methylene chloride solution is washed with water, dried over sodium sulfate and evaporated to afford the title product as an oil.

1. customis prepared
2. temperaturemaintained under a nitrogen atmosphere
3. customAfter two hours reaction time the paste
4. dissolutionredissolves
5. customNext, most of the THF is removed under vacuum
6. dissolutionthe residue dissolved in methylene chloride
7. washThe methylene chloride solution is washed with water
8. dry with materialdried over sodium sulfate
9. customevaporated