3.11. Mycalin B 2

KOH (excess) was added to a stirred solution of 1 (2.5 mg, 0.044 mmol) in MeOH (0.5 mL). After 10 min AcOH was added up to neutrality. The mixture was taken to dryness, the residue was partitioned between water and EtOAc and the organic phase was dried and evaporated. HPLC separation of the crude (eluent: n-hexane-EtOAc, 8:2) gave pure 2 (1.5 mg, 70%) as a colourless oil. 2: For the [α]D20, IR and MS (mass spectrometry) data see refs. 5 and 8. ¹H-NMR: (400 MHz, CDCl₃): δ 4.60 (1H, bd, J = 2.4), 4.55 (1H, bd, J = 2.1), 4.51 (1H, bd, J = 2.2), 4.39 (1H, dd, J = 8.9, 2.0), 4.24 (1H, bd, J = 8.9), 4.13 (1H, ddd, J = 12.7, 9.6, 4.4), 3.73 (1H, ddd, J = 12.2, 9.9, 4.5), 3.58 (1H, dd, J = 9.5, 2.0), 3.38 (1H, ddd, J = 9.5, 9.5, 2.3), 3.00 (1H, ddd, J = 12.8, 4.3, 4.3), 2.59 (1H, d, J = 2.1), 2.44 (1H, ddd, J = 12.3, 12.3, 12.3), 2.38 (1H, dd, J = 10.6, 2.9), 2.10 (1H, dd, J = 10.6, 2.3), 2.04 (1H, m), 1.52 (1H, m), 0.92 (3H, t, J = 7.3). ¹³C-NMR: (100 MHz, CDCl₃): δ 86.0, 83.9, 81.0, 80.7, 79.5, 76.5, 76.1, 73.6, 56.1, 47.5, 46.5, 45.1, 36.6, 25.8, 9.8.