HRID2167321

反应详情

EQUATION

反应方程式

HRID 2167321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In ethanol (5.0 mL), was combined 4-phenoxybenzonitrile (200 mg, 1.02 mmol) and hydroxylamine (250 μL, 4.09 mmol). The mixture was refluxed for 3 hours. The reaction was cooled and then concentrated in vacuo to give the product, which was taken to the next step without further purification (quantitative yield). 1H NMR (500 MHz, CDCL3) δ(ppm): 4.87 (2H, bs), 7.01 (2H, d, J=9.0 Hz), 7.03 (2H, dd, J=8.7, 1.1 Hz), 7.15 (2H, tt, J=7.4, 1.1 Hz), 7.36 (2H, dd, J=8.6, 7.3 Hz), 7.59 (2H, d, J=9.0 Hz). 13C NMR (125 MHz, CDCL3) δ(ppm): 118.6 (CH), 119.6 (CH), 124, 127.3, 127.6 (CH), 130.1 (CH), 152.5, 156.6, 159.3. MS (FAB+): 229 (MH+). HRMS for C13H12N2O2 (MH+): calculated: 229.0977; found 229.0977.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 3 hours
  2. temperatureThe reaction was cooled
  3. concentrationconcentrated in vacuo
  4. customto give the product, which
  5. customwas taken to the next step without further purification (quantitative yield)