HRID270084

反应详情

EQUATION

反应方程式

HRID 270084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2,4-dihydroxyphenyl)ethanone (4.5 g, 29.6 mmol) was dissolved in pyridin (17 mL). Hydroxylamine hydrochloride (2.1 g, 29.6 mmol) was added in small portions over 10 minutes. After stirring at room temperature over night the green-yellowish solution was partitioned between water and ethyl acetate. The organic phase was washed twice with water and once with 0.2 M hydrochloric acid, and was finally concentrated. The oily residue was treated with water, evaporated to yield a white semi solid residue, which was treated with toluene and evaporated to give the titled compound (4.8 g, 98%) as a white solid.

WORKUP

后处理

  1. customwas partitioned between water and ethyl acetate
  2. washThe organic phase was washed twice with water and once with 0.2 M hydrochloric acid
  3. concentrationwas finally concentrated
  4. additionThe oily residue was treated with water
  5. customevaporated
  6. customto yield a white semi solid residue, which
  7. customevaporated