反应详情

温度

90 °C

To a stirred solution of 2,6-dichloro-3,5-dimethoxyaniline (500 g, 2.252 mmol) in dioxane (10 mL) was added 20% phosgene in toluene (4.4 mL, 9.0 mmol) under argon atmosphere at 0° C. The resulting mixture was stirred for 6 h at 90° C., and then allowed to cool to room temperature. The solvents were removed and the residue was dissolved in toluene (10 mL). To this, was added N4-(4-(2-methoxyethoxy)-2-nitrophenyl)-N6-methylpyrimidine-4,6-diamine (0.718 g, 8.358 mmol, 1.0 eq). The resultant reaction mixture was then refluxed for 6 h. After completion of the reaction by TLC (Hexanes:EtOAc, 7:3), reaction mixture was cooled to room temperature, concentrated under vacuum to obtain a crude reaction mixture. The solid precipitated on addition of ethyl acetate to the crude reaction mixture was filtered, washed with ether and pentane to afford the title compound (0.285, yield: 32%) as a white solid. MS (ESI): 567.0 [M+H]+.

1. temperatureto cool to room temperature
2. customThe solvents were removed
3. dissolutionthe residue was dissolved in toluene (10 mL)
4. customThe resultant reaction mixture
5. temperaturewas then refluxed for 6 h
6. customAfter completion of the reaction
7. temperaturewas cooled to room temperature
8. concentrationconcentrated under vacuum
9. customto obtain a crude
10. customreaction mixture
11. customThe solid precipitated on addition of ethyl acetate to the crude
12. customreaction mixture
13. filtrationwas filtered
14. washwashed with ether and pentane