反应详情

To a suspension of 4-hydroxybenzaldehyde (488 mg, 4 mmol) and 6-bromo-1,1,1-trifluorohexane (657 mg, 3 mmol) in MeCN (10 mL) was added K2CO3 (829 mg, 6.00 mmol). The resulting mixture was reflux overnight. Insoluble material was filtered off and rinsed with MeCN. The combined filtrate was concentrated to afford a white solid. This white solid was partitioned between EtOAc and 1 N NaOH solution. The organic layer was separated, washed with sat'd NH4Cl, dried over MgSO4, filtered and concentrated to afford Intermediate 8A as a clear liquid. LCMS Anal. Calc'd for C13H15F3O2 260.10, found [M+H] 261.0.

1. temperatureThe resulting mixture was reflux overnight
2. filtrationInsoluble material was filtered off
3. washrinsed with MeCN
4. concentrationThe combined filtrate was concentrated
5. customto afford a white solid
6. customThis white solid was partitioned between EtOAc and 1 N NaOH solution
7. customThe organic layer was separated
8. washwashed with sat'd NH4Cl
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationconcentrated