反应详情

温度

0 °C

50.6 ml (2 mol/l tetrahydrofuran solution) of isopropylmagnesium chloride was cooled with ice, and a solution having 19.8 g (84.3 mmol) of crude 4-iodo-2-methoxypyridine obtained in Step (c) dissolved in 80 ml of tetrahydrofuran was added, followed by stirring at 0° C. for 1 hour and then at room temperature for 1 hour to prepare 2-methoxy-4-pyridylmagnesium chloride. Then, 16.9 g (127 mmol) of N-chlorosuccinimide was gradually added, followed by stirring at room temperature for 1 hour. 100 ml of water was added to terminate the reaction, and tetrahydrofuran was distilled off under reduced pressure. After extraction with ethyl ether, the organic layer was dried over sodium sulfate and subjected to filtration, and the solvent was distilled off under reduced pressure to obtain 11.0 g (crude yield: 91%) of crude 4-chloro-2-methoxypyridine.

1. additionwas added
2. stirringby stirring at room temperature for 1 hour
3. customto terminate
4. customthe reaction, and tetrahydrofuran
5. distillationwas distilled off under reduced pressure
6. extractionAfter extraction with ethyl ether
7. dry with materialthe organic layer was dried over sodium sulfate
8. filtrationsubjected to filtration
9. distillationthe solvent was distilled off under reduced pressure