methyl 2-methyl-3-(methylamino)propanoate

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:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 16 g of phosgene in 70 ml of toluene, a solution of 17.4 g of methyl 2-methyl-3-methylaminopropionate in 30 ml of toluene was added dropwise with stirring at 20° C. The mixture was stirred at room temperature for 4 hours and evaporated to dryness. The residue was stirred for 10 min. with 100 ml of ethyl ether, filtered, the filtrates are evaporated to dryness and the residue was distilled at high vacuum to give the N-methyl-N-(2-methoxycarbonylpropyl)carbamoyl chloride, bp. 97°-100°/1 mm Hg. The mixture was stirred at room temperature for 4 hours evaporated to dryness The residue was stirred for 10 min. with 100 ml of ethyl ether filtered the filtrates are evaporated to dryness the residue was distilled at high vacuum

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 16 g of phosgene in 70 ml of toluene, a solution of 17.4 g of methyl 2-methyl-3-methylaminopropionate in 30 ml of toluene was added dropwise with stirring at 20° C. The mixture was stirred at room temperature for 4 hours and evaporated to dryness. The residue was stirred for 10 min. with 100 ml of ethyl ether, filtered, the filtrates are evaporated to dryness and the residue was distilled at high vacuum to give the N-methyl-N-(2-methoxycarbonylpropyl)carbamoyl chloride, bp. 97°-100°/1 mm Hg. The mixture was stirred at room temperature for 4 hours evaporated to dryness The residue was stirred for 10 min. with 100 ml of ethyl ether filtered the filtrates are evaporated to dryness the residue was distilled at high vacuum

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

実験手順: To a solution of 12.4 g of methylamine in 45 ml of methanol was added with stirring and ice-water cooling a solution of 60.2 g of methyl 2-methylacrylate in 40 ml of methanol over a period of 1 hour. The mixture was allowed to stand at room temperature for 3 days, was evaporated and the residue was distilled at aspirator pressure to give the methyl 2-methyl-3-methylaminopropionate, bp. 57°-59° C./15 mm Hg. was evaporated the residue was distilled at aspirator pressure

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

実験手順: To a solution of 12.4 g of methylamine in 45 ml of methanol was added with stirring and ice-water cooling a solution of 60.2 g of methyl 2-methylacrylate in 40 ml of methanol over a period of 1 hour. The mixture was allowed to stand at room temperature for 3 days, was evaporated and the residue was distilled at aspirator pressure to give the methyl 2-methyl-3-methylaminopropionate, bp. 57°-59° C./15 mm Hg. was evaporated the residue was distilled at aspirator pressure

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 16 g of phosgene in 70 ml of toluene, a solution of 17.4 g of methyl 2-methyl-3-methylaminopropionate in 30 ml of toluene was added dropwise with stirring at 20° C. The mixture was stirred at room temperature for 4 hours and evaporated to dryness. The residue was stirred for 10 min. with 100 ml of ethyl ether, filtered, the filtrates are evaporated to dryness and the residue was distilled at high vacuum to give the N-methyl-N-(2-methoxycarbonylpropyl)carbamoyl chloride, bp. 97°-100°/1 mm Hg. The mixture was stirred at room temperature for 4 hours evaporated to dryness The residue was stirred for 10 min. with 100 ml of ethyl ether filtered the filtrates are evaporated to dryness the residue was distilled at high vacuum

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

実験手順: To a solution of 12.4 g of methylamine in 45 ml of methanol was added with stirring and ice-water cooling a solution of 60.2 g of methyl 2-methylacrylate in 40 ml of methanol over a period of 1 hour. The mixture was allowed to stand at room temperature for 3 days, was evaporated and the residue was distilled at aspirator pressure to give the methyl 2-methyl-3-methylaminopropionate, bp. 57°-59° C./15 mm Hg. was evaporated the residue was distilled at aspirator pressure