HRID1698538

反应详情

EQUATION

反应方程式

HRID 1698538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2.00 g (8.32 mmol) of methyl 2-[(2-hydroxyethyl)amino]-3-nitrobenzoate in 150 mL of THF was added dropwise 6N HCl (100 mL) at 0° C. and the mixture was stirred for 30 min. The reaction mixture was refluxed for 16 h. After being cooled to room temperature, the mixture was diluted with water (150 ml), and concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with aqueous sodium hydrogen sulfate and water. The organics was dried over magnesium sulfate, filtered, and concentrated in vacuo to give 1.03 g (5.00 mmol, 60%) of the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 16 h
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with aqueous sodium hydrogen sulfate and water
  5. dry with materialThe organics was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo