ethyl 3-piperidin-4-ylpropanoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 3-(piperid-4-yl)propionate (7 g) (prepared similarly to Preparation 21 A using ethyl alcohol in place of methyl alcohol) was dissolved in ethanolic methylamine (33%, 50 ml) and heated in a stainless steel bomb for 6 hours at 120°. The mixture was then evaporated to dryness in vacuo and the residue partitioned between 2 N NaOH (20 ml) and chloroform (40 ml). The chloroform layer was dried (Na2CO3) and evaporated to give N-methyl-3-(piperid-4-yl)propionamide (6 g) as a crude oil. The mixture was then evaporated to dryness in vacuo the residue partitioned between 2 N NaOH (20 ml) and chloroform (40 ml) The chloroform layer was dried (Na2CO3) evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 54 parts of (phenylmethyl)carbonochloridate, 60 parts of ethyl 4-piperidinepropanoate, 31.8 parts of sodium carbonate and 600 parts of trichloromethane was stirred overnight at room temperature. Water was added and the layers were separated. The organic layer was dried, filtered and evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (99:1 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 71 parts (74%) of ethyl 1-(phenylmethoxycarbonyl)-4-piperidinepropanoate as a residue (interm. 1). the layers were separated The organic layer was dried filtered evaporated The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (99:1 by volume) as eluent The pure fractions were collected the eluent was evaporated