反应详情

To a solution of the ester from Step A (120 g, 71.4 mmol) in dry THF (230 mL) at 0° C. was added LAH (2.99 g, 78.6 mmol) portionwise over 30 min. The mixture was stirred for 2 h at room temperature then cooled back to 0° C. and H2O (4.2 mL) was added (care|) dropwise. This was followed by the dropwise addition of 10.6 mL of 1N NaOH then the resulting slurry was stirred at room temperature for 1 h. After filtration through celite washing with EtOAc, the solvent was removed to give the title compound as a clear oil (8.16 g). 1H NMR (CD3OD): δ 1.84 (2H, pentet), 2.68 (2H, t), 3.58 (2H, t), 6.88 (1H, s), 7.80 (1H, s).

1. temperaturethen cooled back to 0° C.
2. stirringthe resulting slurry was stirred at room temperature for 1 h
3. filtrationAfter filtration
4. washthrough celite washing with EtOAc
5. customthe solvent was removed