HRID75841

反应详情

EQUATION

反应方程式

HRID 75841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4-(benzyloxy)benzaldehyde (12.9 g) in MeOH (129 ml), Hydroxylamine hydrochloride (6.34 g) was added and the reaction mixture was refluxed for 3 hours and then cooled. The reaction mixture was concentrated to obtain pale brown residue. To this residue, water was added and it was extracted with EtOAc. Organic layer was collected, dried over Na2SO4 and concentrated to obtain off white solid, which was crystallized from DCM-Petroleum ether to obtain the title compound as white solid. Yield: 11.5 g (83%); 1HNMR (DMSO-d6; 300 MHz): δ 10.98 (s, 1H), 8.06 (s, 1H), 7.53 (d, 2H), 7.33-7.46 (m, 5H), 7.05 (d, 2H), 5.13 (s, 2H).

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 3 hours
  2. temperaturecooled
  3. concentrationThe reaction mixture was concentrated
  4. customto obtain pale brown residue
  5. extractionit was extracted with EtOAc
  6. customOrganic layer was collected
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated
  9. customto obtain off white solid, which
  10. customwas crystallized from DCM-Petroleum ether