反应详情

To a cooled (0° C.) mixture of 1.598 g (3.91 mmol) of methyl 3-hydroxy-2-[(4-methoxybenzenesulfonyl)-(2-amino-5-methylbenzyl)amino]propionate and 1.97 g (19.5) mmol) of triethylamine in 15 ml of dichloromethane was added 0.787 ml (8.60 mmol) of methoxyacetylchloride. The mixture was stirred at room temperature overnight. The mixture was then diluted with CH2Cl2 and washed with H2O, 2 N citric acid, H2O, brine and dried with Na2SO4. The solution was filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated to give 1.94 g of crude methyl 2-{[2-(methoxyacetylamino)-5-methylbenzyl]-(4-methoxy-benzene-sulfonyl)-amino}acrylate as a brown oil. Mass spectrum (ES) 463.4 (M+H).

1. temperatureTo a cooled
2. washwashed with H2O, 2 N citric acid, H2O, brine
3. dry with materialdried with Na2SO4
4. filtrationThe solution was filtered through a thin pad of hydrous magnesium silicate
5. concentrationthe filtrate concentrated