“…The aqueous solution was washed with CH2C12 (5x2 mL), and the combined organic extracts were washed with brine (10 mL) and dried (MgS04). The solvent was removed in vacuo to give a yellow solid, which was chromatographed on silica gel (20:1 ethyl acetate/ methanol) to afford 2 as colorless crystals (20.7 mg, 39%): mp 177-9 °C; NMR (CDC13) 5 3.69 (m, 4 H), 3.76 (m, 4 H), 3.84 (m, 4 H), 4.22 (m, 4 H), 6.94 (d, J = 7.8 Hz, 2 ), 7.07 (dt, Jd = 1 Hz, Jt = 7.7 Hz, 2 ), 7.40 (dt, Jd = 2 Hz, Jt = 7.8 Hz, 2 H), 8.15 (dd, J = 2 Hz, J = 7.8 Hz, 2 ), 8.70 (bs, 2 H); IR (CHC13) 3395,1645 cm"1; CIMS m/z (relative intensity) 415 (M+ + 1,100). Crystals of 2 suitable for X-ray crystallographic studies were obtained from hexanes/CH2C12 (1:1) by the isothermal distillation technique, mp 185-186.5 °C.…”