反应详情

In 20 ml. of dimethylformamide, 1.65 g. of 2-amino-3,5-dichloropyridine was dissolved and 1.0 g. of powdery potassium hydroxide was gradually added with stirring. After the addition, 2.7 g. of 2,6-dinitro-4-trifluoromethylchlorobenzene was added at 30° C. during 5 minutes and the reaction was continued for about 3 hours. The reaction mixture was acidified with conc. HCl and the product was extracted with methylenechloride. The extracted layer was washed with water and dehydrated. The solvent was distilled off and the product was separated by a silica gel column with an eluent of toluene and the solvent was distilled off to obtain 2.8 g. of the object compound having the melting point of 85° to 87° C.

1. additionAfter the addition, 2.7 g
2. extractionthe product was extracted with methylenechloride
3. washThe extracted layer was washed with water
4. distillationThe solvent was distilled off
5. customthe product was separated by a silica gel column with an eluent of toluene
6. distillationthe solvent was distilled off
7. customto obtain 2.8 g