(2H)chlorane

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

実験手順: 38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d=1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 34.8 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C. by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was vaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point--3 mm/Hg: 132°-134° C.). provided with a stirrer reached 54° C. by the end of the introduction to return to ambient temperature The mixture was stirred for one hour filtered the residue was distilled

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

実験手順: 38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d=1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 34.8 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C. by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was vaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point--3 mm/Hg: 132°-134° C.). provided with a stirrer reached 54° C. by the end of the introduction to return to ambient temperature The mixture was stirred for one hour filtered the residue was distilled

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

実験手順: 38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d=1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 34.8 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C. by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was vaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point--3 mm/Hg: 132°-134° C.). provided with a stirrer reached 54° C. by the end of the introduction to return to ambient temperature The mixture was stirred for one hour filtered the residue was distilled

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

実験手順: 38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d = 1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 38.4 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was evaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point - 3 mm/Hg: 132°-134° C). provided with a stirrer reached 54° C by the end of the introduction to return to ambient temperature The mixture was stirred for one hour filtered the solvent was evaporated in vacuo the residue was distilled

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

実験手順: 38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d=1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 34.8 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C. by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was vaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point--3 mm/Hg: 132°-134° C.). provided with a stirrer reached 54° C. by the end of the introduction to return to ambient temperature The mixture was stirred for one hour filtered the residue was distilled