反应详情

Sodium hydride (60% in mineral oil, 1.08 g, 27 mmol) was washed 3× with hexanes then a solution of 4-chloro-2-methylphenol (3.50 g, 24.5 mmol) dissolved in tetrahydrofuran (40 mL) was added. The solution was stirred for 20 minutes then 2-chloro-3-methyl-5-nitropyridine (4.02 g, 23.3 mmol) was added and the reaction mixture was heated to reflux for 3 hours. After cooling, the mixture was concentrated in vacuo then dissolved in ethyl acetate and washed with water, 3× with saturated NaHCO3− and saturated NaCl then dried over Na2SO4 and concentrated in vacuo.

1. additionwas added
2. temperaturethe reaction mixture was heated
3. temperatureto reflux for 3 hours
4. temperatureAfter cooling
5. concentrationthe mixture was concentrated in vacuo
6. dissolutionthen dissolved in ethyl acetate
7. washwashed with water, 3× with saturated NaHCO3− and saturated NaCl
8. dry with materialthen dried over Na2SO4
9. concentrationconcentrated in vacuo