1-piperidin-1-ylprop-2-en-1-one

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in CH2Cl2 (50 ml) was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, dried the clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off dried the clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in 50 ml of CH2Cl2 was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a H2O bath at 60° C. without vacuum. Once most solvent had been evaporated off, it was furthered dried to a clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a H2O bath at 60° C. without vacuum Once most solvent had been evaporated off it was furthered dried to a clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in CH2Cl2 (50 ml) was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a water bath at 60° C. without vacuum. Once most solvent had been evaporated off, dried the clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a water bath at 60° C. without vacuum Once most solvent had been evaporated off dried the clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in CH2Cl2 (50 ml) was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a water bath at 60° C. without vacuum. Once most solvent had been evaporated off, dried the clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a water bath at 60° C. without vacuum Once most solvent had been evaporated off dried the clear oil under high vacuum at RT for 30 min.

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 0° C. solution of acryloyl chloride (4.576 g, 50.558 mmol) in CH2Cl2 (50 ml) was added dropwise and very carefully piperidine (4.305 g, 50.558 mmol). The reaction flask was vented during the exothermic addition. After the addition was completed, the white slurry was stirred at 0° C. for 40 min and at RT for 1 h. The reaction was diluted with 70 ml CH2Cl2 and washed first with about 60 ml 2N HCl and then with about 60 ml of a mix of 2 N NaOH and brine. The organic layer was dried over Na2SO4. The solution was evaporated by heating in a water bath at 60° C. without vacuum. Once most solvent had been evaporated off, dried the clear oil under high vacuum at RT for 30 min. The reaction flask was vented during the exothermic addition After the addition washed first with about 60 ml 2N HCl with about 60 ml of a mix of 2 N NaOH and brine The organic layer was dried over Na2SO4 The solution was evaporated by heating in a water bath at 60° C. without vacuum Once most solvent had been evaporated off dried the clear oil under high vacuum at RT for 30 min.