Reaktion #1857922

Reaktionsgleichung

urea

2-((2-amino-2-methylpropyl)amino)ethanol

ammonia

→

white solid

Ausbeute 41.7%

1-(2-hydroxyethyl)-4,4-dimethylimidazolidin-2-one

Ausbeute 41.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe crude mixture was purified by column chromatography
2. 2
   Wascheneluting from silica gel with a gradient of 0-10% methanol in dichloromethane

Vorschrift

A mixture of urea (5.4 g, 91 mmol) and 2-((2-amino-2-methylpropyl)amino)ethanol (12 g, 91 mmol) was heated in a 200° C. sand bath for approximately 45 min until ammonia evolution had ceased. The crude mixture was purified by column chromatography, eluting from silica gel with a gradient of 0-10% methanol in dichloromethane to give 6.0 g of a white solid. 1H NMR (CDCl3, 400 MHz) δ 1.33 (s, 6H), 3.21 (s, 2H), 3.27-3.30 (t, J=5.2, 2H), 3.69-3.71 (q, J=5.2 Hz, 2H), 4.01-4.04 (t, J=5.4, 1H), 5.31 (br s, 1H); LRMS (ESI/APCI) m/z 159 [M+H]+.

Quelle