反应详情

The material from Example 1A (2.0 mmol) was dissolved in THF (10 mL). DIBAL-H (1 M in hexane, 6 mL, 6.0 mmol) was added. The reaction mixture was stirred at ambient temperature for 30 minutes. Saturated sodium potassium tartrate solution was added slowly at 0° C., followed by addition of diethyl ether. The mixture was stirred vigorously overnight. The organic phase was separated and washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure to provide titled compound (489 mg). MS (ESI(−)) m/e 259 (M−H)+; 1H NMR (300 MHz, DMSO-d6) δ 7.79(t, J=1.7 Hz, 1H), 7.57 (dt, J1=1.7 Hz, J2=7.8 Hz, 1H), 7.45 (dt, J1=1.7 Hz, J2=7.8 Hz, 1H), 7.12 (t, J=7.8 Hz, 1H), 6.48–6.42 (m, 2H), 4.89 (t, J=5.8 Hz, 1H), 4.11 (m, 2H).

1. stirringThe mixture was stirred vigorously overnight
2. customThe organic phase was separated
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure