Acetic acid--water (1/1) → HCID 18005592, compound

Participants

Reaction Steps

The compound obtained in Step C (4 g, 9.5 mmol) is brought to solution in 40 ml of THF. A mixture of AcOH/H2O (7:3) (40 ml) is then added, and the whole is stirred at room temperature for 2 hours. The reaction mixture is then hydrolysed in a mixture of ice and H2O, extracted with AcOEt and washed with a saturated NaHCO3 solution, and then with a saturated NaCl solution, dried over MgSO4 and concentrated to dryness. The residual solid is then triturated in heptane, and the title product is obtained in the form of white crystals, 2.57 g, in a yield of 89%. IR: 3200 2700 ν(OH); 2230 ν(CN); 1390 and 1152 ν cm−1 (NSO2). NMR (CDCl3): 7.9, s, (1H); 7.75 and 7.55 2d, (4H); 6.55 s (1H); 6.15 d (1H); 3.25d(1H,OH); 3.0,s,(6H).

Provenance & Evidence