Dimethylformamide → 2-(4-aminopiperidin-1-yl)-N-methylacetamide

Temperatur

50 °C

To a solution of 2.0 g (10 mmoles) of piperidine, which as dissolved in DMF, anhydrous, 100 mL, was added 2.8 g (20 mmoles) K2CO3, and 1.2 g (11 mmoles) 2-chloro-N-methylacetamide. After stirring at 50° C. for overnight, the mixture was diluted with 500 mL of EtOAc, washed with brine (3×500 mL), dried over Na2SO4, and solvent was evaporated in vacuum. The resulting residue was treated with 50% TFA/DCM and was stirred at r.t. for 2 hrs, and solvent was evaporated in vacuum. The resulting mixture was purified by prep HPLC to give yellow oil, yield 1.5 g (88%). [M+H] calc'd for C8H17N3O, 172. found 172.

1. washwashed with brine (3×500 mL)
2. dry with materialdried over Na2SO4, and solvent
3. customwas evaporated in vacuum
4. additionThe resulting residue was treated with 50% TFA/DCM
5. stirringwas stirred at r.t. for 2 hrs
6. customsolvent was evaporated in vacuum
7. customThe resulting mixture was purified by prep HPLC
8. customto give yellow oil, yield 1.5 g (88%)

ORD-Eintrag

ord-c6cd05ba0044442f8da2291f80e3f789

Quelldatensatz

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08026234B2