1-azabicyclo[2.2.2]octane-3-thiol

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:0.00; pressure:0.00; stir:

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:0.00; pressure:0.00; stir:

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

実験手順: Sodium methylate (0.5 g) is added to a solution of 3-(acetylthio)quinuclidine (14.5 g) in methanol (150 cc). The reaction mixture is then heated under reflux for 1 hour. Sodium methylate (0.5 g) is added again and the mixture is then heated under reflux for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. Distilled water (40 cc) is added to the residue obtained, followed by acetic acid (approximately 1 cc) to obtain a pH in the region of 8. The mixture obtained is extracted with methylene chloride (3×20 cc). The combined organic phases are dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at 30° C. The brown oil obtained is distilled under reduced pressure (920 Pa); the fraction distilling at about 94° C. is collected. 3-Mercaptoquinuclidine (2.8 g) is thereby obtained. The reaction mixture is then heated under reflux for 1 hour the mixture is then heated under reflux for 2 hours The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C Distilled water (40 cc) is added to the residue obtained to obtain a pH in the region of 8 The mixture obtained is extracted with methylene chloride (3×20 cc) The combined organic phases are dried over sodium sulphate filtered concentrated to dryness under reduced pressure (2.7 kPa) at 30° C The brown oil obtained is distilled under reduced pressure (920 Pa) the fraction distilling at about 94° C. is collected

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

実験手順: Sodium methylate (0.5 g) is added to a solution of 3-(acetylthio)quinuclidine (14.5 g) in methanol (150 cc). The reaction mixture is then heated under reflux for 1 hour. Sodium methylate (0.5 g) is added again and the mixture is then heated under reflux for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. Distilled water (40 cc) is added to the residue obtained, followed by acetic acid (approximately 1 cc) to obtain a pH in the region of 8. The mixture obtained is extracted with methylene chloride (3×20 cc). The combined organic phases are dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at 30° C. The brown oil obtained is distilled under reduced pressure (920 Pa); the fraction distilling at about 94° C. is collected. 3-Mercaptoquinuclidine (2.8 g) is thereby obtained. The reaction mixture is then heated under reflux for 1 hour the mixture is then heated under reflux for 2 hours The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C Distilled water (40 cc) is added to the residue obtained to obtain a pH in the region of 8 The mixture obtained is extracted with methylene chloride (3×20 cc) The combined organic phases are dried over sodium sulphate filtered concentrated to dryness under reduced pressure (2.7 kPa) at 30° C The brown oil obtained is distilled under reduced pressure (920 Pa) the fraction distilling at about 94° C. is collected

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

実験手順: Sodium methylate (0.5 g) is added to a solution of 3-(acetylthio)quinuclidine (14.5 g) in methanol (150 cc). The reaction mixture is then heated under reflux for 1 hour. Sodium methylate (0.5 g) is added again and the mixture is then heated under reflux for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. Distilled water (40 cc) is added to the residue obtained, followed by acetic acid (approximately 1 cc) to obtain a pH in the region of 8. The mixture obtained is extracted with methylene chloride (3×20 cc). The combined organic phases are dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at 30° C. The brown oil obtained is distilled under reduced pressure (920 Pa); the fraction distilling at about 94° C. is collected. 3-Mercaptoquinuclidine (2.8 g) is thereby obtained. The reaction mixture is then heated under reflux for 1 hour the mixture is then heated under reflux for 2 hours The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) at 40° C Distilled water (40 cc) is added to the residue obtained to obtain a pH in the region of 8 The mixture obtained is extracted with methylene chloride (3×20 cc) The combined organic phases are dried over sodium sulphate filtered concentrated to dryness under reduced pressure (2.7 kPa) at 30° C The brown oil obtained is distilled under reduced pressure (920 Pa) the fraction distilling at about 94° C. is collected