4-(4-硫代吗啉基)丁酸甲酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 28.0 g. (0.138 mole) of methyl γ-thiomorpholinobutyrate in 300 ml. of concentrated hydrochloric acid and 250 ml. of water was stirred and heated at reflux for 18 hours. The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone. The solid was filtered, washed with acetone, and dried in vacuo to give 28.2 g. (91%) of the desired product as colorless crystals, m.p. 242°-245°C. heated at reflux for 18 hours The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone The solid was filtered washed with acetone dried in vacuo to give 28.2 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 28.0 g. (0.138 mole) of methyl γ-thiomorpholinobutyrate in 300 ml. of concentrated hydrochloric acid and 250 ml. of water was stirred and heated at reflux for 18 hours. The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone. The solid was filtered, washed with acetone, and dried in vacuo to give 28.2 g. (91%) of the desired product as colorless crystals, m.p. 242°-245°C. heated at reflux for 18 hours The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone The solid was filtered washed with acetone dried in vacuo to give 28.2 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 64.0 g. (0.28 mole) of methyl γ-iodobutyrate, 28.0 g. (0.28 mole) of triethylamine, 28.7 g. (0.28 mole) of thiomorpholine (J. Am. Chem. Soc. 76, 1187 (1954)) and 1 liter of benzene was stirred and heated at 60°-70°C. for 18 hours. After cooling the reaction mixture, the precipitated amine hydroiodide was removed by suction filtration. The benzene solution was evaporated to give a orange-red residue which was vacuum distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g. (50%) of the product as a colorless liquid. A mixture of 64.0 g heated at 60°-70°C. for 18 hours After cooling the reaction mixture the precipitated amine hydroiodide was removed by suction filtration The benzene solution was evaporated to give a orange-red residue which distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 64.0 g. (0.28 mole) of methyl γ-iodobutyrate, 28.0 g. (0.28 mole) of triethylamine, 28.7 g. (0.28 mole) of thiomorpholine (J. Am. Chem. Soc. 76, 1187 (1954)) and 1 liter of benzene was stirred and heated at 60°-70°C. for 18 hours. After cooling the reaction mixture, the precipitated amine hydroiodide was removed by suction filtration. The benzene solution was evaporated to give a orange-red residue which was vacuum distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g. (50%) of the product as a colorless liquid. A mixture of 64.0 g heated at 60°-70°C. for 18 hours After cooling the reaction mixture the precipitated amine hydroiodide was removed by suction filtration The benzene solution was evaporated to give a orange-red residue which distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 28.0 g. (0.138 mole) of methyl γ-thiomorpholinobutyrate in 300 ml. of concentrated hydrochloric acid and 250 ml. of water was stirred and heated at reflux for 18 hours. The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone. The solid was filtered, washed with acetone, and dried in vacuo to give 28.2 g. (91%) of the desired product as colorless crystals, m.p. 242°-245°C. heated at reflux for 18 hours The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone The solid was filtered washed with acetone dried in vacuo to give 28.2 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 28.0 g. (0.138 mole) of methyl γ-thiomorpholinobutyrate in 300 ml. of concentrated hydrochloric acid and 250 ml. of water was stirred and heated at reflux for 18 hours. The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone. The solid was filtered, washed with acetone, and dried in vacuo to give 28.2 g. (91%) of the desired product as colorless crystals, m.p. 242°-245°C. heated at reflux for 18 hours The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone The solid was filtered washed with acetone dried in vacuo to give 28.2 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 64.0 g. (0.28 mole) of methyl γ-iodobutyrate, 28.0 g. (0.28 mole) of triethylamine, 28.7 g. (0.28 mole) of thiomorpholine (J. Am. Chem. Soc. 76, 1187 (1954)) and 1 liter of benzene was stirred and heated at 60°-70°C. for 18 hours. After cooling the reaction mixture, the precipitated amine hydroiodide was removed by suction filtration. The benzene solution was evaporated to give a orange-red residue which was vacuum distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g. (50%) of the product as a colorless liquid. A mixture of 64.0 g heated at 60°-70°C. for 18 hours After cooling the reaction mixture the precipitated amine hydroiodide was removed by suction filtration The benzene solution was evaporated to give a orange-red residue which distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 28.0 g. (0.138 mole) of methyl γ-thiomorpholinobutyrate in 300 ml. of concentrated hydrochloric acid and 250 ml. of water was stirred and heated at reflux for 18 hours. The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone. The solid was filtered, washed with acetone, and dried in vacuo to give 28.2 g. (91%) of the desired product as colorless crystals, m.p. 242°-245°C. heated at reflux for 18 hours The solvents were removed on a rotary evaporator to give a colorless residue which crystallized upon trituration with acetone The solid was filtered washed with acetone dried in vacuo to give 28.2 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 64.0 g. (0.28 mole) of methyl γ-iodobutyrate, 28.0 g. (0.28 mole) of triethylamine, 28.7 g. (0.28 mole) of thiomorpholine (J. Am. Chem. Soc. 76, 1187 (1954)) and 1 liter of benzene was stirred and heated at 60°-70°C. for 18 hours. After cooling the reaction mixture, the precipitated amine hydroiodide was removed by suction filtration. The benzene solution was evaporated to give a orange-red residue which was vacuum distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g. (50%) of the product as a colorless liquid. A mixture of 64.0 g heated at 60°-70°C. for 18 hours After cooling the reaction mixture the precipitated amine hydroiodide was removed by suction filtration The benzene solution was evaporated to give a orange-red residue which distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g