HRID1278434

反应详情

EQUATION

反应方程式

HRID 1278434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Methyl 2,6-dinitrobenzoate (15.0 gm.) is suspended in methanol (500 ml.) and 5% palladium on charcoal (1.5 gm.) added. Reduction is carried out on a Parr apparatus for two hours. The solution is filtered with suction and the catalyst washed with a few ml. of methanol. Removal of the methanol gives a brown crystalline product. Extraction with chloroform (50 ml.) and treatment with Darco® gives the product (10.9 gm. 96% yield, m.p. 78°-79.5°). The thin layer chromatogram (Silica gel, 3% methanol in chloroform) shows the material to be homogeneous.

WORKUP

后处理

  1. filtrationThe solution is filtered with suction
  2. washthe catalyst washed with a few ml
  3. customRemoval of the methanol
  4. customgives a brown crystalline product
  5. extractionExtraction with chloroform (50 ml.) and treatment with Darco®
  6. customgives the product (10.9 gm. 96% yield, m.p. 78°-79.5°)