反应详情

温度

180 °C

Into a pressure flask was added compound 7 (3.5 g, 0.014 mol) and 4-(trifluoromethyl)benzylamine (9.0 g, 0.051 mol) and tetrahydrofuran (30.0 mL, 0.37 mol) and palladium acetate (200.0 mg, 0.890 mmol) and 2-(di-t-butylphosphino)biphenyl (200.0 mg, 0.67 mmol). The reaction mixture was stirred at 180 Celsius overnight, poured into water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, concentrated. To the residue was added acetic acid (15.0 mL) and H2O (5.0 mL). The reaction mixture was stirred at 100 Celsius for 5 hours and concentrated to remove acetic acid. The residue was then treated with aqueous Na2HCO3 and extracted with ethyl acetate. The organic layer was washed, dried, concentrated and purified to give product 13 (1.0 g, yield=18.5%) as a light yellow solid (M+1=397).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. additionTo the residue was added acetic acid (15.0 mL) and H2O (5.0 mL)
6. stirringThe reaction mixture was stirred at 100 Celsius for 5 hours
7. concentrationconcentrated
8. customto remove acetic acid
9. additionThe residue was then treated with aqueous Na2HCO3
10. extractionextracted with ethyl acetate
11. washThe organic layer was washed
12. customdried
13. concentrationconcentrated
14. custompurified