Ethanol → HCID 67975039, Verbindung

Temperatur

60 °C

4-(2-(4-chloro-3-nitrophenoxy)ethyl)piperidine (2.3 g, 8.1 mmol, 1 eq.) and tin (II) chloride dihydrate (9.1 g, 40.4 mmol, 5 eq.) were placed in EtOH (81 mL). The reaction mixture was heated at 60° C. and stirred for 19 hours. The reaction mixture was then concentrated under reduced pressure and the resulting residue was diluted with ethyl acetate. The organic phase was washed with a 1N NaOH aqueous solution, dried over MgSO4, filtered and concentrated under reduced pressure. The resulting residue was purified by column chromatography on silica gel to afford 2-chloro-5-(2-piperidinoethoxy)aniline (1.9 g, 92%).

1. concentrationThe reaction mixture was then concentrated under reduced pressure
2. additionthe resulting residue was diluted with ethyl acetate
3. washThe organic phase was washed with a 1N NaOH aqueous solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by column chromatography on silica gel

ORD-Eintrag

ord-085051d86bf84922a2c066a0655a764a

Quelldatensatz

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09061999B2