HRID358652

反应详情

EQUATION

反应方程式

HRID 358652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium carbonate (19 g) was added to a stirred suspension of benzoic acid (34 g) in water (600 ml) and the mixture was warmed gently on a steam bath. After 15 minutes, 2-bromo-2'-nitroacetophenone (68 g) and industrial methylated spirit (1 1) were added. The resultant mixture was heated under reflux for 2 hours, stirred without external heating for 1 0 minutes and then rapidly cooled to 0°-5° in an ice/salt bath with agitation. The mixture was kept at this temperature for 90 minutes and the product was collected by filtration and washed with water to give the novel compound 2-(2-nitrophenyl)-2-oxoethyl benzoate, m.p. 77-80°.

WORKUP

后处理

  1. temperaturethe mixture was warmed gently on a steam bath
  2. temperatureunder reflux for 2 hours
  3. temperaturewithout external heating for 1 0 minutes
  4. temperaturerapidly cooled to 0°-5° in an ice/salt bath with agitation
  5. waitThe mixture was kept at this temperature for 90 minutes
  6. filtrationthe product was collected by filtration
  7. washwashed with water