1-[(2S)-2-吡咯烷羰基]-吡咯烷

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

实验步骤: A 1.0 M solution of lithium aluminium hydride in tetrahydrofuran (87 ml, 87 mmol) was added dropwise to a solution of the crude (pyrrolidin-1-yl)-((S)-pyrrolidin-2-yl)methanone (4.89 g, 29 mmol) in tetrahydrofuran (90 ml). The reaction mixture was heated to reflux for 6 h. It was cooled to room temperature. Water (3.6 ml) was added carefully. A 1 N solution of sodium hydroxide (3.6 ml, 3.6 mmol) was added carefully. Water (10.7 ml) was added. The mixture was stirred for 1 h at room temperature. The precipitation was filtered off. The solvent was removed in vacuo to give 2.67 g of (S)-2-((pyrrolidin-1-yl)methyl)pyrrolidine. The reaction mixture was heated to reflux for 6 h The precipitation was filtered off The solvent was removed in vacuo

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

实验步骤: A 1.0 M solution of lithium aluminium hydride in tetrahydrofuran (87 ml, 87 mmol) was added dropwise to a solution of the crude (pyrrolidin-1-yl)-((S)-pyrrolidin-2-yl)methanone (4.89 g, 29 mmol) in tetrahydrofuran (90 ml). The reaction mixture was heated to reflux for 6 h. It was cooled to room temperature. Water (3.6 ml) was added carefully. A 1 N solution of sodium hydroxide (3.6 ml, 3.6 mmol) was added carefully. Water (10.7 ml) was added. The mixture was stirred for 1 h at room temperature. The precipitation was filtered off. The solvent was removed in vacuo to give 2.67 g of (S)-2-((pyrrolidin-1-yl)methyl)pyrrolidine. The reaction mixture was heated to reflux for 6 h The precipitation was filtered off The solvent was removed in vacuo

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

实验步骤: A 1.0 M solution of lithium aluminium hydride in tetrahydrofuran (87 ml, 87 mmol) was added dropwise to a solution of the crude (pyrrolidin-1-yl)-((S)-pyrrolidin-2-yl)methanone (4.89 g, 29 mmol) in tetrahydrofuran (90 ml). The reaction mixture was heated to reflux for 6 h. It was cooled to room temperature. Water (3.6 ml) was added carefully. A 1 N solution of sodium hydroxide (3.6 ml, 3.6 mmol) was added carefully. Water (10.7 ml) was added. The mixture was stirred for 1 h at room temperature. The precipitation was filtered off. The solvent was removed in vacuo to give 2.67 g of (S)-2-((pyrrolidin-1-yl)methyl)pyrrolidine. The reaction mixture was heated to reflux for 6 h The precipitation was filtered off The solvent was removed in vacuo

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

实验步骤: (S)-2-(Pyrrolidin-1-ylcarbonyl)pyrrolidine-1-carboxylic acid tert-butyl ester (5.90 g, 22 mmol) was dissolved in dichloromethane (50 ml) Trifluoroacetic acid (30 ml) was added. The reaction mixture was stirred for 50 min at room temperature. The solvent was removed in vacuo. The residue was dissolved in a saturated aqueous solution of potassium carbonate (200 ml). It was extracted with dichloromethane (3×100 ml). The aqueous phase was saturated with sodium chloride and extracted with dichloromethane (3×200 ml). The combined organic layers were dried over magnesium sulphate. The solvent was removed in vacuo to give 4.89 g of the crude (pyrrolidin-1-yl)-((S)-pyrrolidin-2-yl)methanone, which was used in the next step without further purification. was added The solvent was removed in vacuo The residue was dissolved in a saturated aqueous solution of potassium carbonate (200 ml) It was extracted with dichloromethane (3×100 ml) extracted with dichloromethane (3×200 ml) The combined organic layers were dried over magnesium sulphate The solvent was removed in vacuo