Triethylamine → HCID 86627037, compound

Participants

Reaction Conditions

Reaction Steps

To 11 L of dehydrated ethyl acetate solution containing 2.45 Kg (8.54 mol) of potassium 4,4-diethoxy-2-ethoxycarbonylbutanoate obtained in Reference example 15-(a) were added 1.63 Kg (17.1 mol) of anhydrous magnesium chloride and 3.12 L (22.2 mol) of triethylamine under argon atmosphere, and the mixture was stirred at 75° C. for 1 hour. Then, 974 g (8.97 mol) of methoxyacetyl chloride was added dropwise to the mixture at 15° C. or lower under cooling in ice-bath, and the mixture was further stirred at room temperature for 6 hours. After completion of the reaction, the reaction mixture was poured into 10 L of ice-water, neutralized with 20% aqueous potassium hydrogen sulfate solution and extracted with ethyl acetate. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 1.68 kg (purity: 66.4%) of the title compound as a yellowish oil. (Yield: 47.3%)

Provenance & Evidence