反应详情

A solution of 10 g (0.048 mol) of 3,4-bis(chloromethyl)-2,5-dimethylthiophene and 8.22 g of p-toluenesulphonamide in 600 ml of dry dimethylformamide is added dropwise, over 6 h, to a stirred suspension, heated to 100°-110° C., of 180 g of potassium carbonate in 900 ml of dimethylformamide. After the end of the addition, the mixture is maintained at the same temperature for 30 min, and then filtered. The solid is washed with dimethylformamide. The filtrate is concentrated under vacuum, and the residue is treated with 100 ml of ethanol, and filtered. The solid residue remaining is washed with ethanol and dried. 9.39 g of product are obtained. Melting point: 163°-164° C.

1. additionAfter the end of the addition
2. temperaturethe mixture is maintained at the same temperature for 30 min
3. filtrationfiltered
4. washThe solid is washed with dimethylformamide
5. concentrationThe filtrate is concentrated under vacuum
6. additionthe residue is treated with 100 ml of ethanol
7. filtrationfiltered
8. washThe solid residue remaining is washed with ethanol
9. customdried