反応 #4699

反応方程式

p-anisidine

4-dimethylamino-benzoic acid chloride

phosphorus pentasulfide

→

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

収率 63.5%

溶媒

pyridine

反応条件

後処理

1. 1
   温度the mixture was refluxed for one hour
2. 2
   温度was refluxed for 2 hours
3. 3
   ろ過filtered
4. 4
   洗浄the 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
   ろ過filtered
8. 8
   洗浄The product was washed with water
9. 9
   その他dried

実験手順

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.

出典