HRID2413522

反应详情

EQUATION

反应方程式

HRID 2413522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.15 g of salicylic acid and 0.03 g of 9-methylphenazinium methylsulphate are placed into a reactor and dissolved in 100 ml of water acidified by acetic acid to the pH=3.0; then 3.0 ml of hydrazine hydrate and 0.5 g of Raney nickel are added thereto. Thereafter, the reaction mixture is maintained for 4 hours under vigorous stirring. Then nickel is filtered-off, the resulting mixture is evaporated to 10 ml and extracted with chloroform. After cooling the precipitated desired product is crystallized by a mixture of water and ethanol in the ratio of 1:1 to give 0.13 g of 2,3-dihydroxybenzoic acid (90% as calculated for the starting compound) having m.p. 203°-204° C. The composition, in %, is as follows:

WORKUP

后处理

  1. temperatureThereafter, the reaction mixture is maintained for 4 hours under vigorous stirring
  2. customthe resulting mixture is evaporated to 10 ml
  3. extractionextracted with chloroform
  4. temperatureAfter cooling the
  5. customprecipitated desired product
  6. customis crystallized by a mixture of water and ethanol in the ratio of 1:1