Hydrochloric Acid → 4-(5-Methylpyridin-3-yl)butan-1-amine

To a solution of 1-(5-methylpyridin-3-yl)butan-1-one (800 mg, 4.9 mmol) and ammonium formate (1.55 g, 24.5 mmol) in methanol (5 mL) under nitrogen was added dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer (45 mg, 0.074 mmol). The solution was heated at reflux for 8 h. after which time the solution was cooled to room temperature and acidified to pH ˜2 with 2M HCl. The mixture was washed with dichloromethane (3×15 mL) and the aqueous phase then basified to pH ˜12 by addition of solid KOH. The aqueous phase was extracted with dichloromethane (3×15 mL) and the combined organic layers washed with brine, dried (Na2SO4) and concentrated to give a pure product (620 mg, 77%).

1. temperatureThe solution was heated
2. temperatureat reflux for 8 h. after which time the solution
3. washThe mixture was washed with dichloromethane (3×15 mL)
4. additionthe aqueous phase then basified to pH ˜12 by addition of solid KOH
5. extractionThe aqueous phase was extracted with dichloromethane (3×15 mL)
6. washthe combined organic layers washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated

ORDレコード

ord-6c4a241115ae4706bb6ffbc1b9609e2a

出典データセット

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07981900B2