Reaktion #169071

Reaktionsgleichung

1,2-Diamino-2-methylpropane

4-chloro-3-nitro[1,5]naphthyridine

triethylamine

→

N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine

Ausbeute 97.4%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated under reduced pressure
2. 2
   Temperaturheated
3. 3
   Temperaturat reflux
4. 4
   workup.STIRRINGwith stirring for 1 hour
5. 5
   TemperaturThe reaction mixture was cooled
6. 6
   Filtrationfiltered
7. 7
   WaschenThe isolated solid was washed with water
8. 8
   Sonstigedried under high vacuum

Vorschrift

1,2-Diamino-2-methylpropane (8.4 mL, 80.0 mmol) was added to a chilled (0° C.) solution of 4-chloro-3-nitro[1,5]naphthyridine (15.2 g, 72.7 mmol) and triethylamine (20.2 mL, 145 mmol) in dichloromethane (350 mL). The reaction mixture was stirred overnight and then concentrated under reduced pressure. The residue was combined with water (300 mL) and heated at reflux with stirring for 1 hour. The reaction mixture was cooled and filtered. The isolated solid was washed with water and then dried under high vacuum to provide 18.5 g of N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine as a bright yellow powder.

Quelle