反应详情

To a suspension of sodium hydride (989 mg, 24.47 mmol) in anhydrous DMF (60 mL) was added portion wise triphenylmethanethiol. After 15 minutes of stirring, ethyl 5-bromovalerate (2.8 mL, 17.48 mmol) was injected and the mixture was stirred at ambient conditions for 24 h. The reaction mixture was portioned between ether and saturated ammonium chloride. The water phase was extracted several times with ether. The recombined organic layer was washed with brine, dried, filtered and evaporated. The crude was flashed using 5–10% ethyl acetate in hexanes. 1H-NMR(CDCl3, 400 MH: 1.23(t, J=7.0 Hz, 3H); 1.42(m, 2H); 1.59(m, 2H); 2.16(m, 4H); 4.09(q, J=7.0 Hz, 2H), 7.21–7.30, 7.42(m, 15H).

1. stirringthe mixture was stirred at ambient conditions for 24 h
2. extractionThe water phase was extracted several times with ether
3. washThe recombined organic layer was washed with brine
4. customdried
5. filtrationfiltered
6. customevaporated