HRID59258

反应详情

EQUATION

反应方程式

HRID 59258 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 4-chloro benzonitrile (1.000 g, 7.26 mmol) in ethanol (20 mL) was added hydroxyl amine HCl (0.752 g, 10.90 mmol) and potassium carbonate (3.00 g, 21.80 mmol). The reaction mass was refluxed for 10-12 h. Excess of solvent was removed under vacuum and the residue was diluted with water, acidified with dilute HCl. Precipitate obtained was filtered off and sucked dried to afford 0.500 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 5.88 (br s, 2H), 7.42 (d, J=8.1 Hz, 2H), 7.68 (d, J=8.4 Hz, 2H), 9.70 (br s, 1H); MS (m/z): 171.13 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mass was refluxed for 10-12 h
  2. customExcess of solvent was removed under vacuum
  3. additionthe residue was diluted with water
  4. customPrecipitate obtained
  5. filtrationwas filtered off
  6. customsucked dried