반응 #324122

반응 방정식

Methyl 2,6-dinitrobenzoate

→

Methyl 2,6-diaminobenzoate

수율 96.0%

용매

chloroform

methanol

methanol

반응 조건

후처리

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

실험 절차

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.

출처