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9 条反应 · 9 篇文献
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 1-(methylsulfonyl)piperidine-4-carboxylate 18 was reacted with lithium aluminum hydride in THF to give 19.
来源 ID: ord-b5bc7ddce0724dbd8ab61f15955d17b8反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 1-(methylsulfonyl)piperidine-4-carboxylate 18 was reacted with lithium aluminum hydride in THF to give 19.
来源 ID: ord-b5bc7ddce0724dbd8ab61f15955d17b8反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of dimethylsulfoxide (39 ml, 0.55 mole) in dichloromethane (300 ml) was added slowly to a solution of oxalyl chloride (22.7 ml, 0.264 mole) in dichloromethane (700 ml) at −60° C. After 10 minutes a solution of 1-methanesulfonylpiperidine-4-methanol (46 grams. 0.238 mole) in dichloromethane (500 ml) was added slowly. After 30 minutes at −60° C., triethylamine (167 ml) was added. The mixture was concentrated under reduced pressure and the residue was partitioned between ethyl acetate (1.2 liters) and water (200 ml). The organic phase was dried (anhydrous magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate/hexane to give 1-methanesulfonylpiperidine-4-carboxaldehyde (34 grams), m.p. 97° C. The mixture was concentrated under reduced pressure the residue was partitioned between ethyl acetate (1.2 liters) and water (200 ml) The organic phase was dried (anhydrous magnesium sulfate) concentrated under reduced pressure The residue was recrystallized from ethyl acetate/hexane
来源 ID: ord-17a21b5be76149768f8a603b6672d50d反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1.0 M lithium aluminum hydride (200 ml, 0.2 mole) in tetrahydrofuran was added dropwise to a solution of 1-methanesulfonylpiperidine-4-carboxylic acid ethyl ester (68 grams, 0.29 mole) in tetrahydrofuran (500 ml) at about +5° C. The reaction mixture was stirred at 5-10° C. for 15 minutes. Water (10 ml) was added dropwise and the mixture was filtered. The filtrate was concentrated under reduced pressure and triturated with 50% ethyl ether-hexane (100 ml). The resulting white solid was collected and dried to give 1-methanesulfonylpiperidine-4-methanol (46 grams, 82%), m.p. 96-97° C. the mixture was filtered The filtrate was concentrated under reduced pressure triturated with 50% ethyl ether-hexane (100 ml) The resulting white solid was collected dried
来源 ID: ord-cc3d3a4026a64e65a09748f3365d0819反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1.0 M lithium aluminum hydride (200 ml, 0.2 mole) in tetrahydrofuran was added dropwise to a solution of 1-methanesulfonylpiperidine-4-carboxylic acid ethyl ester (68 grams, 0.29 mole) in tetrahydrofuran (500 ml) at about +5° C. The reaction mixture was stirred at 5-10° C. for 15 minutes. Water (10 ml) was added dropwise and the mixture was filtered. The filtrate was concentrated under reduced pressure and triturated with 50% ethyl ether-hexane (100 ml). The resulting white solid was collected and dried to give 1-methanesulfonylpiperidine-4-methanol (46 grams, 82%), m.p. 96-97° C. the mixture was filtered The filtrate was concentrated under reduced pressure triturated with 50% ethyl ether-hexane (100 ml) The resulting white solid was collected dried
来源 ID: ord-cc3d3a4026a64e65a09748f3365d0819反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 1-(methylsulfonyl)piperidine-4-carboxylate 18 was reacted with lithium aluminum hydride in THF to give 19.
来源 ID: ord-b5bc7ddce0724dbd8ab61f15955d17b8反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of dimethylsulfoxide (39 ml, 0.55 mole) in dichloromethane (300 ml) was added slowly to a solution of oxalyl chloride (22.7 ml, 0.264 mole) in dichloromethane (700 ml) at −60° C. After 10 minutes a solution of 1-methanesulfonylpiperidine-4-methanol (46 grams. 0.238 mole) in dichloromethane (500 ml) was added slowly. After 30 minutes at −60° C., triethylamine (167 ml) was added. The mixture was concentrated under reduced pressure and the residue was partitioned between ethyl acetate (1.2 liters) and water (200 ml). The organic phase was dried (anhydrous magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate/hexane to give 1-methanesulfonylpiperidine-4-carboxaldehyde (34 grams), m.p. 97° C. The mixture was concentrated under reduced pressure the residue was partitioned between ethyl acetate (1.2 liters) and water (200 ml) The organic phase was dried (anhydrous magnesium sulfate) concentrated under reduced pressure The residue was recrystallized from ethyl acetate/hexane
来源 ID: ord-17a21b5be76149768f8a603b6672d50d反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1.0 M lithium aluminum hydride (200 ml, 0.2 mole) in tetrahydrofuran was added dropwise to a solution of 1-methanesulfonylpiperidine-4-carboxylic acid ethyl ester (68 grams, 0.29 mole) in tetrahydrofuran (500 ml) at about +5° C. The reaction mixture was stirred at 5-10° C. for 15 minutes. Water (10 ml) was added dropwise and the mixture was filtered. The filtrate was concentrated under reduced pressure and triturated with 50% ethyl ether-hexane (100 ml). The resulting white solid was collected and dried to give 1-methanesulfonylpiperidine-4-methanol (46 grams, 82%), m.p. 96-97° C. the mixture was filtered The filtrate was concentrated under reduced pressure triturated with 50% ethyl ether-hexane (100 ml) The resulting white solid was collected dried
来源 ID: ord-cc3d3a4026a64e65a09748f3365d0819反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 1-(methylsulfonyl)piperidine-4-carboxylate 18 was reacted with lithium aluminum hydride in THF to give 19.
来源 ID: ord-b5bc7ddce0724dbd8ab61f15955d17b8PubChem References
以下资料来自该化合物的公开数据库参考记录。