反应详情

A mixture of methyl 3-(5-fluoro-2-nitrophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate (0.51 g, 1.4 mmol), 2,4-dichloro-3-methylphenol (0.33 g, 1.9 mmol) and potassium carbonate (0.28 g, 2.0 mmol) in N,N-dimethylformamide is stirred overnight at room temperature and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extracts are combined, washed sequentially with water, M sodium hydroxide solution, water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a yellow solid. The solid is slurried with an ether/hexanes (1:1) solution, filtered and dried in vacuo to give the title product as a yellow solid, mp 199.9°-202° C.

1. extractionThe aqueous mixture is extracted with ethyl acetate
2. washwashed sequentially with water, M sodium hydroxide solution, water and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customto obtain a yellow solid
6. filtrationfiltered
7. customdried in vacuo