反应详情

4-chloro-3,5-dinitrotoluene (9.0 gm.) is dissolved in 50% ethanol (30 ml.). Electrolytically reduced iron powder (14.2 gm.) is added and the stirred reaction mixture heated to reflux. Concentrated HCl (1 ml.) in 50% ethanol (5 ml.) is added dropwise and refluxing continued for one hour. The reaction mixture is allowed to cool slightly and made basic (pH 8) with 20% NaOH, then the iron removed by filtration. The filtrate is taken to dryness under reduced pressure and the residue extracted with hot Skellysolve "B" (700 ml.). The product precipitates in long needles that were collected by filtration (4.57 gm., m.p. 114°-115.5°, 70% yield).

1. customthe stirred reaction mixture
2. temperatureheated to reflux
3. temperaturerefluxing
4. temperatureto cool slightly
5. customthe iron removed by filtration
6. extractionthe residue extracted with hot Skellysolve "B" (700 ml.)
7. customThe product precipitates in long needles that
8. filtrationwere collected by filtration (4.57 gm., m.p. 114°-115.5°, 70% yield)