反应详情

温度

-78 °C

2,2,6,6-Tetramethylpiperidine (3.0 g) was added dropwise to a stirred solution of n-butyllithium (1.6M in hexanes, 13 mL) in dry tetrahydrofuran (12 mL) at −78° C. After 10 min, 2-(4-fluorophenyl)ethanol (1.00 g) was added dropwise. The reaction mixture was stirred at −78° C. for 5 h and then dry DMF (3.18 mL) was added dropwise over 5 min. The cooling bath was removed and the reaction mixture allowed to warm to room temperature overnight. Ethyl acetate and aqueous HCl (2M) were added and the solution separated. The ethyl acetate layer was washed with water, brine, dried over sodium sulphate, filtered and evaporated in vacuo. Purification was by silica gel chromatography eluting with ethyl acetate:isohexane, 1:1 to give the subtitled compound as an oil. Yield 0.43 g.

1. customThe cooling bath was removed
2. temperatureto warm to room temperature overnight
3. additionEthyl acetate and aqueous HCl (2M) were added
4. customthe solution separated
5. washThe ethyl acetate layer was washed with water, brine
6. dry with materialdried over sodium sulphate
7. filtrationfiltered
8. customevaporated in vacuo
9. customPurification
10. washeluting with ethyl acetate