1-Piperazinecarboxylic acid, ethyl ester → HCID 86679353, compound

Participants

Reaction Steps

Ethyl 4-fluoro-3-nitrobenzoate (10.0 g, 46.91 mmol) prepared in the Step 1-1-1 was dissolved in ethanol (100 ml). To the solution, triethylamine was added and then ethoxycarbonylpiperazine (49.26 mmol) was added, and the mixture was stirred at a room temperature for 18 hours. After the mixture was concentrated, ethyl acetate was added thereto. The resulting mixture was washed with a saturated sodium bicarbonate solution and a saturated saline solution in order. The washed product was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1-1:1) to give the title compound (17.4 g, quantitative) as a yellowish-brown oily substance.

Provenance & Evidence