4-吗啉基丁腈

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

实验步骤: A mixture of 10.0 g of 4-bromobutyronitrile, 14.7 g of morpholine and 40 g of tetrahydrofuran was heated under reflux for 10 hours. The reaction solution was cooled, diluted with diethyl ether, filtered, and concentrated in vacuum. Purification by vacuum distillation yielded 9.4 g of 4-morpholinobutyronitrile (boiling point: 85° C./50 Pa, yield: 91%). was heated under reflux for 10 hours The reaction solution was cooled filtered concentrated in vacuum Purification by vacuum distillation

反应条件: temp:-55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 14.8 g lithium aluminium hydride were weighed under N2 atmosphere into a round-bottomed flask. The substance was cooled down to −55° C. and 150 ml ether was added dropwise. The suspension was allowed to stir; then 30 g 4-Morpholin-4-yl-butyronitrile were dissolved in 200 ml ether and the solution was added dropwise to the reaction mixture. Again 200 ml ether were added to the mixture and the reaction was stirred at room temperature overnight. At the next day the mixture was cooled down to less than 10° C. and 35 ml H2O were added carefully. After five hours the mixture was fritted and the residue was washed with 300 ml ether. The filtrate was dried, concentrated and finally distilled under vacuum. The product fractions were collected at 74-78° C. and 2.1-1.6 Torr. The purity of the colourless oil was judged by gas chromatography, GC-MS and 1H-NMR. the solution was added dropwise to the reaction mixture the reaction was stirred at room temperature overnight At the next day the mixture was cooled down to less than 10° C. the residue was washed with 300 ml ether The filtrate was dried concentrated finally distilled under vacuum The product fractions were collected at 74-78° C.

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 196.9 ml morpholine, 500 ml toluol and 100 ml chloroform were stirred in a round-bottomed flask under N2 atmosphere and at 80° C. After one hour 100 g 4-chlorobutyronitrile was added dropwise within one hour. The reaction was stirred one day at 80° C. and another day at room temperature. The mixture was fritted and the residue was washed two times with ether. The filtrate was concentrated and finally distilleed under vacuum. The product fractions were collected at 95-100° C. and 1.2-0.89 Torr. The purity of the colourless oil was judged by gas chromatography and 1H-NMR. the residue was washed two times with ether The filtrate was concentrated The product fractions were collected at 95-100° C.

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

实验步骤: A mixture of 10.0 g of 4-bromobutyronitrile, 14.7 g of morpholine and 40 g of tetrahydrofuran was heated under reflux for 10 hours. The reaction solution was cooled, diluted with diethyl ether, filtered, and concentrated in vacuum. Purification by vacuum distillation yielded 9.4 g of 4-morpholinobutyronitrile (boiling point: 85° C./50 Pa, yield: 91%). was heated under reflux for 10 hours The reaction solution was cooled filtered concentrated in vacuum Purification by vacuum distillation

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

实验步骤: A mixture of 10.0 g of 4-bromobutyronitrile, 14.7 g of morpholine and 40 g of tetrahydrofuran was heated under reflux for 10 hours. The reaction solution was cooled, diluted with diethyl ether, filtered, and concentrated in vacuum. Purification by vacuum distillation yielded 9.4 g of 4-morpholinobutyronitrile (boiling point: 85° C./50 Pa, yield: 91%). was heated under reflux for 10 hours The reaction solution was cooled filtered concentrated in vacuum Purification by vacuum distillation

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To anhydrous THF (70 mL) was added LiAlH4 (5.37 g, 142 mmol) in one portion. The mixture was stirred at 0° C. for 20 min, and a solution of 4-morpholinobutanenitrile (7.26 g, 47 mmol) in anhydrous THF (40 mL) was added dropwise. Upon the end of addition the mixture was refluxed for 4 h, then cooled to 0° C., diluted with water (20 mL) and filtered. The filtrate was concentrated in vacuo to give the crude product for the next step without further purification. Upon the end of addition the mixture was refluxed for 4 h cooled to 0° C. filtered The filtrate was concentrated in vacuo

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

实验步骤: To a suspension of K2CO3 (8.28 g, 60 mmol) and morpholine (4.35 g, 50 mmol) in acetonitrile (50 mL) was added 4-bromobutyronitrile (7.40 g, 50 mmol) dropwise at rt under N2. The mixture was stirred at rt for 6 h, filtered and concentrated in vacuo to give the title compound (7.26 g, 94.2%). filtered concentrated in vacuo

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To anhydrous THF (70 mL) was added LiAlH4 (5.37 g, 142 mmol) in one portion. The mixture was stirred at 0° C. for 20 min, and a solution of 4-morpholinobutanenitrile (7.26 g, 47 mmol) in anhydrous THF (40 mL) was added dropwise. Upon the end of addition the mixture was refluxed for 4 h, then cooled to 0° C., diluted with water (20 mL) and filtered. The filtrate was concentrated in vacuo to give the crude product for the next step without further purification. Upon the end of addition the mixture was refluxed for 4 h cooled to 0° C. filtered The filtrate was concentrated in vacuo

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

实验步骤: To a suspension of K2CO3 (8.28 g, 60 mmol) and morpholine (4.35 g, 50 mmol) in acetonitrile (50 mL) was added 4-bromobutyronitrile (7.40 g, 50 mmol) dropwise at rt under N2. The mixture was stirred at rt for 6 h, filtered and concentrated in vacuo to give the title compound (7.26 g, 94.2%). filtered concentrated in vacuo

反应条件: temp:-55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 14.8 g lithium aluminium hydride were weighed under N2 atmosphere into a round-bottomed flask. The substance was cooled down to −55° C. and 150 ml ether was added dropwise. The suspension was allowed to stir; then 30 g 4-Morpholin-4-yl-butyronitrile were dissolved in 200 ml ether and the solution was added dropwise to the reaction mixture. Again 200 ml ether were added to the mixture and the reaction was stirred at room temperature overnight. At the next day the mixture was cooled down to less than 10° C. and 35 ml H2O were added carefully. After five hours the mixture was fritted and the residue was washed with 300 ml ether. The filtrate was dried, concentrated and finally distilled under vacuum. The product fractions were collected at 74-78° C. and 2.1-1.6 Torr. The purity of the colourless oil was judged by gas chromatography, GC-MS and 1H-NMR. the solution was added dropwise to the reaction mixture the reaction was stirred at room temperature overnight At the next day the mixture was cooled down to less than 10° C. the residue was washed with 300 ml ether The filtrate was dried concentrated finally distilled under vacuum The product fractions were collected at 74-78° C.

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 196.9 ml morpholine, 500 ml toluol and 100 ml chloroform were stirred in a round-bottomed flask under N2 atmosphere and at 80° C. After one hour 100 g 4-chlorobutyronitrile was added dropwise within one hour. The reaction was stirred one day at 80° C. and another day at room temperature. The mixture was fritted and the residue was washed two times with ether. The filtrate was concentrated and finally distilleed under vacuum. The product fractions were collected at 95-100° C. and 1.2-0.89 Torr. The purity of the colourless oil was judged by gas chromatography and 1H-NMR. the residue was washed two times with ether The filtrate was concentrated The product fractions were collected at 95-100° C.

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

实验步骤: A mixture of 10.0 g of 4-bromobutyronitrile, 14.7 g of morpholine and 40 g of tetrahydrofuran was heated under reflux for 10 hours. The reaction solution was cooled, diluted with diethyl ether, filtered, and concentrated in vacuum. Purification by vacuum distillation yielded 9.4 g of 4-morpholinobutyronitrile (boiling point: 85° C./50 Pa, yield: 91%). was heated under reflux for 10 hours The reaction solution was cooled filtered concentrated in vacuum Purification by vacuum distillation