反应详情

A mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride solution, dried (MgSO4) and concentrated in vacuo to give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C.

1. temperatureis heated at 50°-55° for 30 minutes
2. extractionThe resultant mixture is extracted with ethyl acetate
3. washThe combined extracts are washed with a saturated sodium chloride solution
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give an orange oil residue
7. temperaturecooled
8. filtrationfiltered
9. customto give an orange solid filtercake
10. customRecrystallization of the solid from isopropanol