Trifluoroacetic acid → HCID 89534609, compound

Participants

Reaction Steps

To a mixture of 1.0 g of N′-(2,2-dimethoxyethyl)-N,N-diethylethane-1,2-diamine, 0.84 mL of N-ethyl-N-isopropylpropan-2-amine, and 10 ml of methylene chloride was added 0.70 mL of ethyl succinyl chloride under ice cooling, followed by stirring for 1 hour under ice cooling. The reaction mixture was concentrated under reduced pressure, ethyl acetate and water were added thereto, and extracted with ethyl acetate. The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate, followed by concentration under reduced pressure, thereby obtaining 1.2 g as oily product. A mixture of 1.2 g of the obtained oily product, 12 mL of methylene chloride, and 12 mL of trifluoroacetic acid (TFA) was stirred for 4 hours at room temperature. The reaction mixture was concentrated under reduced pressure, an aqueous sodium hydrogen carbonate solution and ethyl acetate were added thereto, and extracted with ethyl acetate. The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate, followed by concentration under reduced pressure, thereby obtaining 0.78 g of ethyl 4-{[2-(diethylamino)ethyl](2-oxoethyl)amino}-4-oxobutanoate.

Provenance & Evidence