反应详情

温度

25 °C

To a solution of trimethyl acetic acid (9.98 g, 97.7 mmol) in methylene chloride (200 ml) cooled to 0° C. is added 4-aminobenzyl amine (11.1 ml, 97.7 mmol), triethyl amine (34.1 ml, 244 mmol), HOAt (13.3 g, 97.7 mmol), and EDC (18.73 g, 97.7 mmol). The reaction mixture is allowed to slowly warm to 25° C. and stirred at this temperature for 18 hrs. The reaction mixture is diluted with water and the organic layer is extracted, washed with aqueous sodium bicarbonate and brine, dried over magnesium sulfate and concentrated in vacuo. The crude product is purified by flash chromatography (silica gel, 40% to 65% ethyl acetate in hexane) to give N-(4-amino-benzyl)-2,2-dimethyl-propionamide (16.8 g), as a pale yellow solid.

1. extractionthe organic layer is extracted
2. washwashed with aqueous sodium bicarbonate and brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe crude product is purified by flash chromatography (silica gel, 40% to 65% ethyl acetate in hexane)