ethyl 2-piperidin-2-ylacetate;hydrochloride

Conditions: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Ethyl 2-(pyridin-2-yl)acetate (24.51 g, 148.4 mmol) was dissolved in ethanol (130 ml), and PtO2 (3.37 g, 14.84 mmol, 0.1 eq.) and chloroform (20 ml) were added. The suspension was stirred under an H2 atmosphere (8 bar) at 40° C. overnight. According to TLC control (silica gel, MC/methanol 95:5), the reaction was not complete, so that further chloroform (15 ml) was added and the mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control). After cooling, the catalyst was first removed by filtering over filtering earth and the filtrate was concentrated to dryness in vacuo. The ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification. the mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control) After cooling the catalyst was first removed by filtering over filtering earth the filtrate was concentrated to dryness in vacuo The ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification

Conditions: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Ethyl 2-(pyridin-2-yl)acetate (24.51 g, 148.4 mmol) was dissolved in ethanol (130 ml), and PtO2 (3.37 g, 14.84 mmol, 0.1 eq.) and chloroform (20 ml) were added. The suspension was stirred overnight under a H2 atmosphere (8 bar) at 40° C. According to TLC monitoring (silica gel, DCM/methanol 95:5), the reaction was incomplete, so that further chloroform (15 ml) was added and stirring was carried out for a further 2 d under a H2 atmosphere (8 bar) at 40° C. (TLC monitoring). After cooling, the catalyst was first removed by filtration over filtering earth and the filtrate was concentrated to dryness in vacuo. The ethyl 2-(piperidin-2-yl)acetate hydrochloride was used in the next stage without being purified further. Yield: 31.51 g, >100% was added stirring was carried out for a further 2 d under a H2 atmosphere at 40° C. After cooling the catalyst was first removed by filtration over filtering earth the filtrate was concentrated to dryness in vacuo without being purified further