反应详情

温度

120 °C

10 g of 3-methylsulfanylbenzoic acid and 0.05 ml of DMF were suspended in 50 ml of DCM. 9 ml of thionyl chloride were added and the mixture was heated under reflux for 4 h. The volatiles were removed in vacuo and the residue was taken up in 30 ml of toluene and transferred to a pressure bottle. 180 ml of a 0.5 M solution of ammonia in dioxane were added, the bottle was sealed and the mixture was heated to 120° C. for 5 h. The solvent was removed in vacuo and the residue taken in water and EA. The phases were separated and the aqueous layer was extracted with EA. The combined organic phases were washed with brine and dried over sodium sulfate. The solvent was removed in vacuo. 8.6 g of the title compound were obtained as a brown solid.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 4 h
3. customThe volatiles were removed in vacuo
4. addition180 ml of a 0.5 M solution of ammonia in dioxane were added
5. customthe bottle was sealed
6. customThe solvent was removed in vacuo
7. customThe phases were separated
8. extractionthe aqueous layer was extracted with EA
9. washThe combined organic phases were washed with brine
10. dry with materialdried over sodium sulfate
11. customThe solvent was removed in vacuo