反应详情

To a solution of 2-tert-butyl-4-fluoro-5-nitrophenyl methyl carbonate (C-7-a) (1.08 g, 4 mmol) in CH2Cl2 (40 mL) was added piperidine (3.94 mL, 10 mmol). The mixture was stirred at room temperature for 1 h and extracted with 1N NaOH (3×). The aqueous layer was acidified with 1N HCl and extracted with diethyl ether. The ether extract was washed with brine, dried (MgSO4) and concentrated to give 2-tert-butyl-4-fluoro-5-nitrophenol (530 mg, 62%). 1H NMR (400 MHz, DMSO-d6) δ 10.40 (s, 1H), 7.49 (d, J=6.8 Hz, 1H), 7.25 (d, J=13.7 Hz, 1H), 1.36 (s, 9H).

1. extractionextracted with 1N NaOH (3×)
2. extractionextracted with diethyl ether
3. extractionThe ether extract
4. washwas washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated