HRID2273669

反应详情

EQUATION

反应方程式

HRID 2273669 的结构方程式

PROCEDURE

实验过程

This compound was prepared, starting from compound 105 (1.00 g, 2.32 mmol), according to the procedure developed for compound 102. Reaction time at 200° C.: 2 h, reaction time at 140° C.: 5 h; the purification was performed using column chromagraphie (Al2O3, CH2Cl2/EtOH, 99/1, v/v) to give compound 106 (458 mg, 1.10 mmol) as a yellow solid. Yield 48%; Rf (Al2O3, CH2Cl2/EtOH, 99/1, v/v) 0.42; mp 58-60° C.; IR (KBr) ν 1342, 1486, 1518, 1555, 1681, 2760, 2966, 3385 cm−1; 1H NMR (200 MHz, CDCl3) δ 1.06 (t, 6H, J=7.1 Hz), 2.56 (q, 4H, J=7.1 Hz), 2.69 (t, 2H, J=6.1 Hz), 3.54 (q, 2H, J=6.1 Hz), 7.76 (dd, 1H, 5JH-F=1.2 Hz, J=8.9 Hz), 7.96 (m, 2H), 8.42 (d, 1H, J=1.7 Hz), 8.50 (m, 1H); ESI-MS m/z 415.9 [M+H]+.

WORKUP

后处理

  1. customThis compound was prepared
  2. customReaction time at 200° C.
  3. custom2 h, reaction time at 140° C.
  4. custom5 h
  5. customthe purification