Reaktion #640583

Reaktionsgleichung

hydrochloric acid water

3-Aminopropanol

triethylamine

2-nitrobenzyl chloride

→

3-(2-nitrobenzylamino)propanol

Ausbeute 33.2%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter heated
2. 2
   Temperaturto reflux for seven hours
3. 3
   Temperaturto cool
4. 4
   Extraktionextracted with ether
5. 5
   Extraktionextracted with ethyl acetate
6. 6
   WaschenThe organic layer was washed with a saturated brine
7. 7
   Trocknendried over anhydrous sodium sulfate
8. 8
   Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

3-Aminopropanol (3.94 g, 52.5 mmol) and triethylamine (1.77 g, 17.5 mmol) were dissolved in tetrahydrofuran (30 ml) and added with 2-nitrobenzyl chloride (3.00 g, 17.5 mmol) at room temperature. After heated to reflux for seven hours, the reaction mixture was allowed to cool and poured into 1N hydrochloric acid water and extracted with ether. The aqueous layer was adjusted to pH 9 with a saturated sodium hydrogen carbonate aqueous solution and then extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 3-(2-nitrobenzylamino)propanol (1.22 g).

Quelle