反应详情

温度

0 °C

Diisobutylaluminium hydride (1.5 M in toluene) (2.12 ml, 3.18×10−3 mole) was added dropwise at 0° C. under nitrogen to a suspension of 5-Cyano-2,6-Diamino-3-(2,3,5-trichlorophenyl)pyrazine (0.5 g, 1.59×10−3 mole) in dry toluene (70 ml) and the reaction was stirred at 0° C. for 1 hr. A further one equivalent of diisobutylaluminium hydride was then added and the mixture again stirred at 0° C. for 1 hr. Methanol (1 ml) was added carefully at 0° C. under nitrogen to destroy excess hydride and the reaction was warmed to room temperature. Ethyl acetate (100 ml) was added and the solution was washed with 5% citric acid solution (2×100 ml). The organic layer was separated, washed with brine (100 ml), dried over magnesium sulphate, filtered and the filtrate evaporated in vacuo to give the desired product. Yield 0.340 g (67%), N.m.r. (D6DMSO) δ: 7.53 (1H, d), 7.91 (1H, d), 6.90-7.80 (4H, b), 9.49 (1H, s).

1. stirringthe mixture again stirred at 0° C. for 1 hr
2. customto destroy excess hydride
3. temperaturethe reaction was warmed to room temperature
4. additionEthyl acetate (100 ml) was added
5. washthe solution was washed with 5% citric acid solution (2×100 ml)
6. customThe organic layer was separated
7. washwashed with brine (100 ml)
8. dry with materialdried over magnesium sulphate
9. filtrationfiltered
10. customthe filtrate evaporated in vacuo