HRID22469

反应详情

EQUATION

反应方程式

HRID 22469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 5-Bromo-o-anisaldehyde (6.45 g), hydroxylamine hydrochloride (2.2 g), sodium acetate (4.1 g) and acetic acid (20 mL) was heated at 100° C. with stirring for 1 h. Acetic anhydride was added (20 mL) and the mixture was refluxed for 8 h. The reaction mixture was poured onto ice water and the mixture was made basic by the careful addition of 50% sodium hydroxide. The product was extracted with ether, the ether extracts were dried over magnesium sulfate and the sovent was removed in vacuo. The residue was crystallized from ether/hexane to afford 5-Bromo-2-methoxybenzonitrile.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 8 h
  2. additionThe reaction mixture was poured onto ice water
  3. extractionThe product was extracted with ether
  4. dry with materialthe ether extracts were dried over magnesium sulfate
  5. customthe sovent was removed in vacuo
  6. customThe residue was crystallized from ether/hexane