反应详情

A solution of 15.9 g 2,4-dichlorobenzoyl chloride in tetrahydrofuran (15 ml) was added dropwise to a solution of 18.67 g ethyl 3-[3-(aminomethyl)-4-methoxyphenyl]-2-isopropoxypropanoate and 7.7 g triethylamine in diethyl ether (300 ml) under ice-cooling. After stirring under ice-cooling for 30 minutes and further at room temperature for 30 minutes, the reaction solution was poured into 500 ml water and extracted with 300 ml ethyl acetate. The organic layer was successively washed with 200 ml saturated aqueous sodium bisulfate, 200 ml saturated sodium hydrogencarbonate and 200 ml brine, dried over anhydrous magnesium sulfate and the solvent was evapoarated. The residue was purified by silica gel column chromatography (eluting solvent: hexane-ethyl acetate), to give 28.2 g of ethyl 3-(3-{[(2,4-dichlorobenzoyl)amino]methyl}-4-methoxyphenyl)-2-isopropoxypropanoate identical in TLC and 1H-NMR to the compound obtained in Example 31g) as a colorless solid.

1. temperaturecooling
2. extractionextracted with 300 ml ethyl acetate
3. washThe organic layer was successively washed with 200 ml saturated aqueous sodium bisulfate, 200 ml saturated sodium hydrogencarbonate and 200 ml brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe residue was purified by silica gel column chromatography (eluting solvent: hexane-ethyl acetate)