反应详情

Sodium hydride in oil (60%, 7.0 g) was added with ice-cooling to a solution of 5-(1-hydroxyethyl)-2-methylpyridine (20.0 g) in N,N-dimethylformamide (120 ml). The mixture was stirred for 15 minutes. Then, chloromethyl methyl ether (14.1 g) was added dropwise at the same temperature. The reaction mixture was further stirred for 30 minutes with ice-cooling. The mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate and subjected to distillation under reduced pressure to obtain 5-(1-methoxymethoxyethyl)-2-methylpyridine (21.5 g, yield: 81%), b.p. 78°-80° C./0.8 mmHg.

1. stirringThe reaction mixture was further stirred for 30 minutes with ice-
2. temperaturecooling
3. extractionextracted with ethyl acetate
4. washThe ethyl acetate layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationsubjected to distillation under reduced pressure