tert-Butanol → HCID 118022810, compound

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Reaction Steps

The title compound of step 2 (1.0 g, 6.1 mmol), diphenylphosphoryl azide (2.64 mL 12.2 mmol), and triethylamine (1.64 mL, 12.2 mmol) in tBuOH (50 mL) under N2 were heated at 80° C. for 2 h. Silica gel chromatography (PE/EtOAc=5:1) gave the title compound (570 mg, 40%) as a white solid. 1H NMR (CDCl3, 300 MHz): δ 8.18 (d, J=4.8 Hz, 1H), 7.04 (d, J=4.8 Hz, 1H), 2.90-2.97 (m, 4H), 2.06-2.12 (m, 2H), 1.49 (s, 9H). LCMS: 235 (M+1)+

Provenance & Evidence