反应详情

温度

130 °C

Benzyl 4-amino-3-methoxybenzoate (1.92 g, 6.8 mmol) and K2CO3 (2.38 g, 17 mmol) are suspended in 4 mL dioxane and then mixed with 2,4-dichloro-5-trifluoromethylpyrimidine (1.48 mL, 6.8 mmol). The suspension is then refluxed for 100 min with stirring in the oil bath (approx. 130° C.). Once the reaction has ended the reaction mixture is filtered, the filtrate is concentrated by rotary evaporation and purified by normal-phase column chromatography. The product-containing fractions of A-3a (HPLC-MS: tRet.=1.94 min; MS (m-H)−=436) are combined and concentrated by rotary evaporation.

1. temperatureThe suspension is then refluxed for 100 min
2. filtrationis filtered
3. concentrationthe filtrate is concentrated by rotary evaporation
4. custompurified by normal-phase column chromatography
5. customThe product-containing fractions of A-3a (HPLC-MS: tRet.=1.94 min; MS (m-H)−=436)
6. concentrationconcentrated by rotary evaporation