HRID339418

反应详情

EQUATION

反应方程式

HRID 339418 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of isoindoline (576 mg, 4.0 mmol) in dry 1,4-dioxane (20 mL) was added 4-methoxy-2-methylphenyl isocyanate (815 mg, 5.0 mmol) under argon at room temperature. The reaction mixture was then stirred at RT overnight. The solvent was evaporated under reduced pressure, and the residue was purified by chromatography on silica gel (EtOAc/hexanes: 1:1) to give the title compound (1.18 g, 84%) as a white solid. 1H NMR (500 MHz, DMSO-d6): δ 2.19 (s, 3H), 3.72 (s, 3H), 4.73 (s, 4H), 6.72 (dd, J=2.5 Hz, 8.5 Hz, 1H), 6.78 (d, J=2.5 Hz, 1H), 7.17 (d, J=8.5 Hz, 1H), 7.30-7.32 (m, 2H), 7.34-7.36 (m, 2H), 7.74 (s, 1H), 13C NMR (DMSO-d6): δ 18.2, 51.9, 55.1, 110.9, 115.1, 122.8, 127.2, 127.8, 130.6, 135.1, 137.0, 154.9, 156.5; MS (MH+, 283); EA calc'd for C17H18N2O2: C, 72.32; H, 6.43; N, 9.92. Found C, 72.16; H, 6.82; N, 9.98.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by chromatography on silica gel (EtOAc/hexanes: 1:1)