“…The resulting orange-brown crystals were collected by filtration, washed repeatedly with water, recrystallized by dissoving in methanol at room temperature, adding water, and chilling to -20°. The resulting orange-yellow crystals (413 mg, 0.90 mmol, 36%) had: ir (CHCL) 3360, 2950, 2860, 2460,1600,1550,1450, 1360,1200,1085, 970 cm-1; deuteriumdecoupled nmr (CDCL) 0.76 (s, 9) 0.78 (obscured), 1.62 (d, 1,7 = 13.1 Hz), 7.1-8.6 (m, 5). A sample of do material prepared in an analogous manner had the following elemental analysis.…”