Triethylamine → HCID 23093475, compound

Participants

Reaction Steps

To a mixture of tert-butyl 2-hydroxyethyl(methyl)carbamate (1.75 g) obtained in Reference Synthetic Example 1 and ethyl acetate (15 mL) was added triethylamine (1.67 mL), and a mixture of trimethylacetyl chloride (1.35 mL) and ethyl acetate (5 mL) was added dropwise. The reaction solution was stirred at room temperature for 2 hrs, then, pyridine (1.62 mL) was added thereto, and stirred overnight at room temperature. To the reaction solution was added ethyl acetate (50 mL), and washed sequentially with water (50 mL), 5% aqueous solution of citric acid (50 mL) and saturated saline (50 mL), and dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure, and to the residue was added 4N hydrogen chloride-ethyl acetate solution (10 mL). After stirring at room temperature for 2 hrs, diethyl ether (10 mL) was added thereto, and the depositting solid was collected by filtration. The solid was dried under reduced pressure to give title compound as white solid (1.65 g).

Provenance & Evidence