Reaktion #1278003

Reaktionsgleichung

(R)-1-[2-formyloxy-5-nitro-6-chloropyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester

methylamine

→

titled product

Ausbeute 75.9%

(R)-1-[2-formyloxy-5-nitro-6-methylaminopyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester

Ausbeute 75.9%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   ExtraktionThe reaction solution was extracted with dichloromethane
3. 3
   Sonstigedried
4. 4
   Sonstigeevaporated to dryness
5. 5
   Sonstigeto afford a crude product as yellow solid, which
6. 6
   Sonstigewas purified through a column chromatography (ethyl acetate:petroleum ether=1:1)

Vorschrift

In a dry reaction bottle, 16 g (R)-1-[2-formyloxy-5-nitro-6-chloropyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester (40 mmol) was added and dissolved in 50 mL ethanol. 31 g 40% methylamine aqueous solution (400 mmol) was added. The stirring was continued for 2 days at 60° C. The reaction solution was extracted with dichloromethane, dried, and evaporated to dryness to afford a crude product as yellow solid, which was purified through a column chromatography (ethyl acetate:petroleum ether=1:1) to afford 12 g titled product with a yield of 75.9%.

Quelle