反应详情

1-Chloro-4-nitronaphthalene (2.00 g, 9.63 mmol), 5-ethylaminomethyl-1-azabicyclo[3.3.0]octane (3.24 g, 19.3 mmol) and sodium iodide (580 mg) were added into anhydrous pyridine (20.0 ml) to react the mixture in a sealed tube for 20 hours at 190° C. After addition of aqueous sodium hydroxide solution subsequent to concentration in vacuo, the reaction mixture was extracted by ethyl acetate, dried over anhydrous sodium sulfate, concentrated in vacuo, and purified by column chromatography to afford the desired compound (1.00 g, 30.6%), as a yellow liquid.

1. customto react the mixture in a sealed tube for 20 hours at 190° C
2. concentrationsubsequent to concentration in vacuo
3. extractionthe reaction mixture was extracted by ethyl acetate
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. custompurified by column chromatography