反应详情

A mixture of 0.50 g of the product of Example 7, 0.2 g 2-phenethyl isocyanate, and a few mL ethyl acetate were briefly heated on the steambath and then allowed to sit 3 days at room temperature. The reaction mixture was then washed with dilute H3PO4, NaHCO3, and HaCl solutions, dried over MgSO4, filtered, and concentrated to an oil. The oil was chromatographed on SiO2 (70-230 mesh) using EtoAc as eluant. The product was obtained as an oil which crystallized on standing. 0.28 g (44%). NMR (CDCl3) δ 0.88 (3H, t), δ 1.25 (24H, m), δ 1.96 (4H, m) δ 2.84 (2H, t), δ 3.23 (2H, t), δ 3.51 (2H, q), δ 3.69 (6H, s), δ 3.77 (3H, s), δ 4.03 (2H, s), δ 4.70 (1H, t), δ 5.35 (2H, t), δ 6.13 (2H, s), δ 7.16-7.31 (5H, m), δ 7.46 (1H, s). IR (KBr) 3251, 2925, 1662, 1621, 1533, 1465, 1156, 1128, 810 cm-1.

1. washThe reaction mixture was then washed with dilute H3PO4, NaHCO3, and HaCl solutions
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated to an oil
5. customThe oil was chromatographed on SiO2 (70-230 mesh)
6. customThe product was obtained as an oil which
7. customcrystallized