反应详情

To a flask were added 50 g polyphosphoric acid. After heating to 70 C under nitrogen, a mixture of 3.13 g 2-aminothiophenol and 1.65 g dimethylmalonic acid was added. The reaction mixture was heated to 150 C for 2 hours, then 165 C for 3 hours. After cooling to 80 C, the mixture was poured into 100 ml water. The slurry was cooled to 5 C, filtered and the solid was washed with water. The solid was added to a mixture of 20 ml ethanol and 210 ml water at 50 C and basified with aqueous ammonium hydroxide. After cooling to 10 C, the solid was filtered and washed with water. The solid was dissolved in 50 ml hot ethanol, hot filtered and 5 ml water was added and the solution was cooled to 5 C. Following filtration, the white solid was washed with 75% ethanol and dried.

1. temperatureAfter heating to 70 C under nitrogen
2. additionwas added
3. temperatureThe reaction mixture was heated to 150 C for 2 hours
4. temperatureAfter cooling to 80 C
5. temperatureThe slurry was cooled to 5 C
6. filtrationfiltered
7. washthe solid was washed with water
8. additionThe solid was added to a mixture of 20 ml ethanol and 210 ml water at 50 C
9. temperatureAfter cooling to 10 C
10. filtrationthe solid was filtered
11. washwashed with water
12. dissolutionThe solid was dissolved in 50 ml hot ethanol
13. filtrationhot filtered
14. addition5 ml water was added
15. temperaturethe solution was cooled to 5 C
16. filtrationfiltration
17. washthe white solid was washed with 75% ethanol
18. customdried