反应详情

Lithium aluminum hydride (132 mg, 3.49 mmol, 2.1 eq.) was added to a solution of 4-[2-(1-pyrrolidinyl)ethoxy]benzamide (389 mg, 1.66 mmol) in dry THF (25 mL) then the reaction heated at reflux for 20 h. The reaction was allowed to cool to ambient temperature then quenched with water (0.250 mL). Aqueous sodium hydroxide (0.250 mL of 15% w/v) then water (0.750 mL) was added and the reaction stirred for 30 min. The reaction mixture was passed through a pad of diatomaceous earth which was washed with THF (3×15 mL). The combined organics were concentrated under reduced pressure to give the amine as oil (372 mg, >100%) which was used without further purification.

1. temperaturethe reaction heated
2. temperatureat reflux for 20 h
3. customthen quenched with water (0.250 mL)
4. additionAqueous sodium hydroxide (0.250 mL of 15% w/v) then water (0.750 mL) was added
5. washwas washed with THF (3×15 mL)
6. concentrationThe combined organics were concentrated under reduced pressure