反应详情

Anhydrous NH3 (g) was bubbled into a stirred solution of ethyl N-nitrocarbamate (503.0 g, 3.75 mol, mp 63°-66° C.), CH2Cl2 (1625 mL) and dry CH3OH (825 mL), precooled to 9° C. under N2, until the exothermic reaction subsided (the NH3 addition rate was controlled so as not to exceed a reaction temperature of 23° C.). After the NH3 addition was complete, the mixture was filtered and the collected solid was dried under high vacuum (overnight) to give ammonium ethyl N-nitrocarbamate as colorless crystals (563.0 g, 99%). mp 175°-176° C. IR (KBr) 3230 (s), 3000 (m), 1725 (s) and 1685 (s), 1445 and 1395 (s), 1310 (m), 1220 (s), 1100 (S), 1030 (m) cm-1. 1H NMR (90 MHz, d6 -DMSO) δ 7.30 (bs, 4H, exch D2O), 3.90 (q, 2H, J=4.5 Hz), 1.10 (t, 3H, J=4.5 Hz).

1. customprecooled to 9° C. under N2, until the exothermic reaction
2. customa reaction temperature of 23° C.
3. filtrationthe mixture was filtered
4. customthe collected solid was dried under high vacuum (overnight)