反应详情

温度

60 °C

To a solution containing 1.52 g of 4-nitro-N-methylaniline (10 mmol) in 30 mL THF, was added 0.8 g of sodium hydride (60% dispension in oil, 20 mmol). After 5 minutes at room temperature, 2.59 g of 2-(dimethylamino)ethyl chloride hydrochloride (18 mmol) and 0.4 g of sodium hydride (60% dispension in oil, 10 mmol) were added. The reaction was heated at 60° C. for 5 hours. The solvent was concentrated in vacuo to yield a residue which was partitioned between ethyl acetate and 2 M sodium hydroxide solution. The organic phase was washed with water (3×), dried over anhydrous sodium sulphate, filtered, and concentrated in vacuo to yield the title compound as a brown oil (1.23 g, 55%). MS (ES+) m/e 224 [M+H]+.

1. concentrationThe solvent was concentrated in vacuo
2. customto yield a residue which
3. customwas partitioned between ethyl acetate and 2 M sodium hydroxide solution
4. washThe organic phase was washed with water (3×)
5. dry with materialdried over anhydrous sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo