反应详情

温度

-78 °C

4-trifluoromethoxy bromobenzene (2.41 g, 10 mmol) was dissolved in dry tetrahydrofuran (30 mL), cooled to −78° C., to which slowly added dropwise n-butyllithium (1.6M n-hexane solution, 6.5 mL), kept the temperature below −70° C. during the dropwise adding procedure, after adding, kept stirring this system for 20 min, added 4-carbonyl piperidine-1-formic acid tert-butyl ester (1.99 g, 10 mmol) in tetrahydrofuran solution, kept the temperature below −70° C. during the dropwise adding procedure, after adding, the temperature can be increased to room temperature while stirring for 15 h. After the reaction was finished, added saturated ammonium chloride aqueous solution to quench reaction, partitioned, organic phases were washed by saturated saline, followed by anhydrous sodium sulphate drying, concentration, column chromatography (PE: EA=15:1) to give 1.6 g light yellow gel-like substance, yield: 40%.

1. customthe temperature below −70° C.
2. additiondropwise adding procedure
3. additionafter adding
4. customthe temperature below −70° C.
5. additiondropwise adding procedure
6. additionafter adding
7. temperaturethe temperature can be increased to room temperature
8. stirringwhile stirring for 15 h
9. customto quench
10. customreaction
11. custompartitioned
12. washorganic phases were washed by saturated saline
13. concentrationfollowed by anhydrous sodium sulphate drying, concentration, column chromatography (PE: EA=15:1)
14. customto give 1.6 g light yellow gel-like substance, yield: 40%