反应详情

温度

110 °C

Step A (Method 1, Using Standard Buchwald Coupling Conditions): To a 10 mL reaction tube fitted with a screw cap is charged with 5-phenylpyrrolidin-2-one (26.8 mg, 0.166 mmol), 1-(4-iodophenoxy)-4-chlorobenzene (66 mg, 0.199 mmol, 1.2 eq), copper iodide (6.3 mg, 0.033 mmol, 0.2 eq), K3PO4 (70.6 mg, 0.333 mmol, 2.0 eq), trans-cyclohexane-1,2-diamine (3.8 mg, 0.033 mmol, 0.2 eq) and 1,4-dioxane (2 mL). The system is degassed with argon then sealed and heated to 110° C. for 20 h. The reaction is cooled to room temperature, dissolved in ethyl acetate and washed with water and brine. The organic phase is dried over Na2SO4, filtered and concentrated in vacuo. Purification on silica gel (0-33% ethyl acetate in hexane) gives 1-[4-(4-chlorophenoxy)phenyl]-5-phenylpyrrolidin-2-one as a slightly brown oil (30.0 mg, 50%).

1. customStep A (Method 1, Using Standard Buchwald Coupling Conditions): To a 10 mL reaction tube
2. customfitted with a screw
3. customcap
4. customThe system is degassed with argon
5. customthen sealed
6. temperatureThe reaction is cooled to room temperature
7. dissolutiondissolved in ethyl acetate
8. washwashed with water and brine
9. dry with materialThe organic phase is dried over Na2SO4
10. filtrationfiltered
11. concentrationconcentrated in vacuo
12. customPurification on silica gel (0-33% ethyl acetate in hexane)