反应详情

To a 100-mL round-bottomed flask was added 9 (1.16 g, 4.67 mmol) suspended in 30 mL phosphorus oxychloride. The reaction mixture was heated at reflux with stirring in an anhydrous atmosphere for 3 h. The dark orange solution was allowed to cool to room temperature and concentrated in vacuo. Water (20 mL) was then added to the residue at 0° C. with vigorous stirring to give an exothermic reaction. Concentrated aqueous ammonium hydroxide was added to pH 5 to give a precipitate, which was collected by filtration, washed with water (3×5 mL), and dried in vacuo. The crude product was purified by silica gel column chromatography with 2% MeOH/CHCl3. Recrystallization from MeOH afforded 1.07 g (86%) of 10 as a white solid: TLC Rf0.35 (MeOH/CHCl3, 1:10); mp 162-163° C.; 1H NMR (DMSO-d6) δ 1.19 (s, 9 H), 2.47 (s, 3 H), 6.33 (s, 1 H), 9.85 (s, 1 H), 12.07 (s, 1 H) Anal. (C12H15ClN4O) C, H, N, Cl.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux
3. concentrationconcentrated in vacuo
4. additionWater (20 mL) was then added to the residue at 0° C.
5. stirringwith vigorous stirring
6. customto give
7. customan exothermic reaction
8. customto give a precipitate, which
9. filtrationwas collected by filtration
10. washwashed with water (3×5 mL)
11. customdried in vacuo
12. customThe crude product was purified by silica gel column chromatography with 2% MeOH/CHCl3
13. customRecrystallization from MeOH