HRID2224653

反应详情

EQUATION

反应方程式

HRID 2224653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-hydroxy-5-methoxybenzaldehyde (4.00 g) in formic acid (30 ml) were added hydroxylamine hydrochloride (2.01 g) and sodium formate (3.22 g) at room temperature and the mixture was refluxed for 2 hours. The reaction mixture was concentrated. the residue was diluted with water and was extracted with t-butyl methyl ether. The extract was washed with water, dried over anhydrous magnesium sulfate and concentrated. The residue was washed with a mixture of t-butyl methyl ether and hexane to give the title compound (2.02 g) having the following physical data.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. concentrationThe reaction mixture was concentrated
  3. additionthe residue was diluted with water
  4. extractionwas extracted with t-butyl methyl ether
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. washThe residue was washed with a mixture of t-butyl methyl ether and hexane