반응 #4699

반응 방정식

p-anisidine

4-dimethylamino-benzoic acid chloride

phosphorus pentasulfide

→

4-dimethylamino-N-(4'-methoxyphenyl)-benzenecarbothiamide

수율 63.5%

용매

pyridine

반응 조건

후처리

1. 1
   온도the mixture was refluxed for one hour
2. 2
   온도was refluxed for 2 hours
3. 3
   여과filtered
4. 4
   세척the product was washed with 0.1N hydrochloric acid
5. 5
   workup.ADDITIONA mixture of the product and 300 ml of N sodium hydroxide solution
6. 6
   workup.STIRRINGwas stirred for one hour
7. 7
   여과filtered
8. 8
   세척The product was washed with water
9. 9
   기타dried

실험 절차

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.

출처