反应详情

温度

30 °C

13.6 g of p-anisidine were added to a solution of 22.2 g of 4-dimethylamino-benzoic acid chloride in 84 ml of anhydrous pyridine and the mixture was refluxed for one hour and cooled to 30° C. 33 g of phosphorus pentasulfide were added to the mixture which was refluxed for 2 hours and was then poured into an ice water-concentrated hydrochloric acid mixture. The mixture was stirred for one hour and was vacuum filtered and the product was washed with 0.1N hydrochloric acid. A mixture of the product and 300 ml of N sodium hydroxide solution was stirred for one hour and was vacuum filtered. The product was washed with water and dried to obtain 13.5 g of 4-dimethylamino-N-(4'-methoxyphenyl)-benzenecarbothiamide melting at 192° C.

1. temperaturethe mixture was refluxed for one hour
2. temperaturewas refluxed for 2 hours
3. filtrationfiltered
4. washthe product was washed with 0.1N hydrochloric acid
5. additionA mixture of the product and 300 ml of N sodium hydroxide solution
6. stirringwas stirred for one hour
7. filtrationfiltered
8. washThe product was washed with water
9. customdried