Hydrochloric Acid → HCID 70237563, compound

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Reaction Steps

2 g (0.0066 mol) of tert-butyl 4-(2-methoxycarbonylmethoxyethyl)piperazine-1-carboxylate prepared in Example I.4.3. are dissolved in 10 ml of ethanol in a 50 ml three-necked round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. 11 ml of a 3.8M solution of hydrochloric acid in ethanol are added in a single portion with stirring. The mixture is stirred at room temperature for 30 minutes and a further 11 ml of a 3.8M solution of hydrochloric acid in ethanol are added. The mixture is brought at the reflux temperature for 4 hours. The solvent is removed on a rotary evaporator under reduced pressure. 1.86 g (97.3%) of ethyl 2-(1-piperazinyl)-ethoxyacetate dihydrochloride are obtained in the form of a pale yellow oil which crystallizes. NMR: δ: 1.21 (3H, t, 7.1 Hz); 3.37 (2H, t, 4.8 Hz); 3.46 (1H, m); 3.55 (4H, m); 3.91 (2H, t, 4.8 Hz); 4.14 (2H, q, 7.1 Hz); 4.18 (2H, s); 10.1 (1H, bs); 12 (1H, bs). Mass spectrum: 216 (M+·).

Provenance & Evidence