反应详情

Hydrogen chloride gas was bubbled through neat ethylcyanoformate (0.997 ml, 10.1 mmol) until the solution became a white solid, approximately 2 hours. The solid was partitioned between CH2Cl2 and water. The CH2Cl2 layer was collected dried (MgSO4) and concentrated to a white solid. The product was crystallized from hot absolute ethanol to give the title compound (m. p. 169-170° C.). 1H NMR (CDCl3)δ 1.42 (t, 9H, 3x CH3), 4.50 (q, 6H, 3x CH2). 13C NMR (DMSO) δ 14.06 (CH3), 64.02 (CH2), 161.27 (CO), 166.86 (Triazine Ar).

1. customa white solid, approximately 2 hours
2. customThe solid was partitioned between CH2Cl2 and water
3. customThe CH2Cl2 layer was collected
4. dry with materialdried (MgSO4)
5. concentrationconcentrated to a white solid
6. customThe product was crystallized from hot absolute ethanol