反应详情

0.400 g (1.10 mmol) of 2,4-dibromo-3-(aminocarbonylmethoxy)benzoic acid, 0.140 g (1.20 mmol) of cyclohexane-1,3-dione, 0.222 g (1.10 mmol) of N′-(3-dimethyl-aminopropyl) -N-ethylcarbodiimide hydrochloride and 0.001 g of DMAP was stirred for 14 hours at RT in 15 ml of CH2Cl2. The mixture was subsequently diluted with CH2Cl2 and with 0.5 N HCl, and washed with water, with saturated NaHCO3 solution and again with water. After the combined organic phases have been dried over Na2SO4 and concentrated completely, 3-oxo-1-cyclohexenyl 2,4-dibromo-3-(aminocarbonylmethoxy)benzoate was obtained as a yellow resin, which had sufficient purity for the subsequent reaction.

1. washwashed with water, with saturated NaHCO3 solution and again with water
2. dry with materialAfter the combined organic phases have been dried over Na2SO4
3. concentrationconcentrated completely