HRID380516

反应详情

EQUATION

反应方程式

HRID 380516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2 g (9.4 mmol) of 2,3-di-nitrobenzoic acid in 20 mL of acetic acid at 0° C. was added a solution of 14.8 g (65 mmol) SnCl2. 2 H2O in 7 mL of concentrated HCl. After stirring for 2 h at rt, the reaction mixture was concentrated. The residue was dissolved in 30 mL of H2O and the pH was adjusted to pH=12-13 with 6N NaOH. The mixture was filtered and the solid was washed with 0.1N HCl. The combined aqueous fractions were concentrated to give 1.4 g of the title compound.

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated
  2. dissolutionThe residue was dissolved in 30 mL of H2O
  3. filtrationThe mixture was filtered
  4. washthe solid was washed with 0.1N HCl
  5. concentrationThe combined aqueous fractions were concentrated