反应详情

3.3 g (0.01 mol) 2-methyl-N-[4-methyl-2-[2-(methylsulfonyl)-4-pyrimidinyl]phenyl]propanamide was dissolved in 35 mL absolute ethanol and 3 g potassium hydrogen sulfide was added to this solution with stirring. The reaction mixture was stirred overnight at room temperature. 50 mL water was added and the volume reduced under vacuum to 40 mL. An additional 40 mL water was added and the solution thus obtained was made acidic with concentrated hydrochloric acid. The yellow precipitate was collected by filtration, washed with a little water, then dissolved in 50 mL 1N sodium hydroxide and treated with charcoal. The charcoal was filtered off and the filtrate was made acidic with concentrated hydrochloric acid. The bright yellow precipitate was collected by filtration, washed with water, then dried in a vacuum oven to yield 2.18 g of N-[2-(2-mercapto-4-pyrimidyl)-4-methylphenyl]-2-methylpropanamide. 1H NMR (CDCl3): δ 1.21 (d,6H), 2.40 (s,3H), 2.75 (m,1H), 7.40-8.60 (5H), 11.4(s,1H,NH), 11.9(s,1H,SH).

1. stirringThe reaction mixture was stirred overnight at room temperature
2. customthe solution thus obtained
3. filtrationThe yellow precipitate was collected by filtration
4. washwashed with a little water
5. dissolutiondissolved in 50 mL 1N sodium hydroxide
6. additiontreated with charcoal
7. filtrationThe charcoal was filtered off
8. filtrationThe bright yellow precipitate was collected by filtration
9. washwashed with water
10. customdried in a vacuum oven