反应详情

温度

95 °C

The final product was synthesized as trifluoroacetate salt starting from (S)-5-(4-propoxyphenyl)morpholin-3-one (0.044 g, 0.19 mmol), 4-iodobenzene-1,2-diamine (0.044 g, 0.19 mmol), copper(I) iodide (0.004 g, 0.019 mmol), cesium fluoride (0.058 g, 0.38 mmol), cyclohexane-1,2-diamine (0.0025 mL, 0.019 mmol). The solids were given together in a reaction flask and the flask was purged with argon. A solution of cyclohexane-1,2-diamine in 2 mL dioxane was added to the flask. The reaction was stirred at 95° C. for 4 days, before the reaction was cooled down to 45° C. and filtered through a pad of celite. The pad was washed with warm dichloromethane and the solution was concentrated under reduced pressure. The intermediate product was purified via FPLC using a chloroform-methanol gradient (0→10%) Yield: 0.01 g (15%); MS m/z 342.2 (M+H)+

1. customThe solids were given together in a reaction flask
2. customthe flask was purged with argon
3. additionA solution of cyclohexane-1,2-diamine in 2 mL dioxane was added to the flask
4. temperaturewas cooled down to 45° C.
5. filtrationfiltered through a pad of celite
6. washThe pad was washed with warm dichloromethane
7. concentrationthe solution was concentrated under reduced pressure
8. customThe intermediate product was purified via FPLC