反应详情

温度

50 °C

9.04 g of hexamethylene tetramine was added to a solution of 10.0 g N1-(2-methoxybenzyl)-2,4-dichlorobenzamide in trifluoroacetic acid (200 mL), followed by stirring at 50° C. for 23 hours. The reaction solution was left and cooled to room temperature and then concentrated. The residue was diluted with ice-water and adjusted to pH 11 to 12 with 1N aqueous sodium hydroxide solution. The solution was extracted with ethyl acetate. The organic layer was washed with 1 N aqueous sodium hydroxide solution (×3), 1 N hydrochloric acid (×2) and brine, dried over anhydrous sodium sulfate and filtered thorough 100 g silica gel. After concentrating the filtrate, the residue was suspended in ethyl acetate. The solid was collected by filtration and washed with ethyl acetate, to give 7.15 g of N1-(5-formyl-2-methoxybenzyl)-2,4-dichlorobenzamide as a colorless solid.

1. waitThe reaction solution was left
2. temperaturecooled to room temperature
3. concentrationconcentrated
4. additionThe residue was diluted with ice-water
5. extractionThe solution was extracted with ethyl acetate
6. washThe organic layer was washed with 1 N aqueous sodium hydroxide solution (×3), 1 N hydrochloric acid (×2) and brine
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered thorough 100 g silica gel
9. concentrationAfter concentrating the filtrate
10. filtrationThe solid was collected by filtration
11. washwashed with ethyl acetate