HRID49033

反应详情

EQUATION

反应方程式

HRID 49033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,3-tetramethylene glutarimide (6.9 mg) and potassium carbonate (40 mg) in dimethylformamide (0.5 mL) was stirred at room temperature for 30 minutes. 1-(2-Chloroethyl)-4-(2-fluorophenyl)piperazine (10.0 mg) was added and the resulting solution was heated at 120° C. for 3 hours. The solvent was removed and the residue was purified by thin-layer chomatography (silica gel, eluting with hexane/ethyl acetate, 1:1), giving the title compound as a white solid (6.2 mg, 40%). 1H NMR (300 MHz, CDCl13) δ7.07-6.87 (m, 4H), 3.96 (t, 2H, J=6.6 Hz), 3.05 (t, 4H, J=4.8 Hz), 2.67 (t, 4H, J=4.7 Hz), 2.59 (s, 4H), 2.54 (t, 4H, J=6.6 Hz), 1.73-1.68 (m, 4H), 1.55-1.50 (m, 4H). ESI-MS m/z 374 (MH+).

WORKUP

后处理

  1. temperaturethe resulting solution was heated at 120° C. for 3 hours
  2. customThe solvent was removed
  3. customthe residue was purified by thin-layer chomatography (silica gel, eluting with hexane/ethyl acetate, 1:1)