反应详情

24 g 2,2-dimethyl-N-[4-methyl-2-[2-(methylthio)-4-pyrimidinyl]phenyl]propanamide was dissolved in 120 mL glacial acetic acid and the mixture warmed to reflux when 60 mL 15% hydrochloric acid solution was gradually added. After the addition was completed, the reaction mixture was heated at reflux for 4 h. After cooling, volatiles were removed in vacuo, the residue was taken up in 200 mL water and ice was added. The resulting mixture was neutralized to pH 10 with 5% sodium hydroxide solution and extracted with ether. Organic extracts were washed with brine, dried, evaporated to dryness and then dried in a vacuum oven to yield 6.2 g of the title compound as a tan solid melting at 120°-123° C. 1H NMR (CDCl3): δ 2.30 (s,3H), 2.60 (s,3H), 5.8 (s,2H,NH2), 6.60-8.6 (5H).

1. temperaturethe mixture warmed
2. additionwas gradually added
3. additionAfter the addition
4. temperaturethe reaction mixture was heated
5. temperatureat reflux for 4 h
6. temperatureAfter cooling
7. customvolatiles were removed in vacuo
8. additionice was added
9. extractionextracted with ether
10. washOrganic extracts were washed with brine
11. customdried
12. customevaporated to dryness
13. customdried in a vacuum oven