Methanesulfonic Acid → HCID 86590437, compound

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Reaction Steps

Compound 26.135 (5.37 g, 9.59 mmol) is dissolved in a mixture of methanol (50 mL) and THF (100 mL), and methanesulfonic acid (921 mg, 9.59 mmol) is added dropwise. The solution is allowed to stand for 15 minutes and then concentrated in vacuo. The pale yellow foam is dissolved in ethanol and concentrated to give 6.3 g (100%) of a pale yellow amorphous solid, mp. 150-156° C. 1H NMR (400 MHz, DMSO-D6): δ=1.79 (s, 3H), 1.96 (m, 2H), 2.30 (s, 3H), 2.64 (t, 2H, J=7.2 Hz), 3.12 (m, 4H), 3.35 (m, 6H), 3.50-3.70 (m, 4H), 4.46 (d, 2H, J=6.8 Hz), 7.02 (s, 1H), 7.26 (d, 2H, J=8.4 Hz), 7.36 (d, 2H, J=8.4 Hz), 7.40-7.48 (m, 3H), 7.87 (brs, 1H), 8.04 (brs, 1H), 8.39 (dd, 2H, J=2.0, 7.2 Hz), 9.68 (brs, 1H), 12.09 (brs, 1H). MS (ES): 560.0/562.0 (100/33) [MH+]. tR (method B)=10.5 min.

Provenance & Evidence