HRID477072

反应详情

EQUATION

反应方程式

HRID 477072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

242 g (1 mole) of 4,4'-dimethoxybenzophenone was suspended in 2,000 ml of ethanol and 210 g (3 mole) of hydroxylamine hydrochloride and 300 ml (3 mole) of a 10N aqueous solution of NaOH were added thereto. Then the obtained mixture was heated under reflux. After two or three hours, the ethanol was distilled off in vacuo and then a saline solution was added thereto followed by extracting with chloroform. The chloroform phase was washed with water and dried over magnesium sulfate. After distilling the chloroform off, the residue was recrystallized from ethanol. Thus 240 g of the title compound was obtained in the form of colorless needles. m.p.: 131° to 132° C.

WORKUP

后处理

  1. temperatureThen the obtained mixture was heated
  2. temperatureunder reflux
  3. distillationAfter two or three hours, the ethanol was distilled off in vacuo
  4. additiona saline solution was added
  5. extractionby extracting with chloroform
  6. washThe chloroform phase was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationAfter distilling the chloroform off, the residue
  9. customwas recrystallized from ethanol