반응 #502120

반응 방정식

2-Hydroxyethylamine

HNO3

Ac2O

→

title compound

2-(Nitrooxy)ethylammonium nitrate

용매

EtOAc

반응 조건

후처리

1. 1
   기타The solvent was evaporated in high vacuo at 40° C
2. 2
   기타The residue was sonicated with ether
3. 3
   여과The solid was filtered
4. 4
   세척washed with hexane

실험 절차

2-Hydroxyethylamine (5 g, 81.9 mmol) in EtOAc (40 mL) was added drop-wise to a mixture of fuming HNO3 (18 g, 12 mL, 0.29 mol) and Ac2O (54 g, 50 mL, 0.53 mol) at −10° C. The reaction mixture was stirred at 0° C. for 10 minutes and at room temperature for 10 minutes. The solvent was evaporated in high vacuo at 40° C. The residue was sonicated with ether. The solid was filtered and washed with hexane to give the title compound as a white solid. Mp 92-94° C. 1H NMR (300 MHz, d6-DMSO) δ 7.71-8.25 (bs, 3H), 4.72 (t, J=5.0 Hz, 2H), 3.23 (d, J=5.0 Hz, 2H). 13C NMR (75 MHz, d6-DMSO) δ 70.9, 37.4.

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