Chloride → HCID 69241294, compound

Participants

Reaction Steps

To a mixture of Example 17C (31.1 g, 0.1 mol) and cobalt (TI) chloride (11.9 g, 0.05 mol) in methanol (300 mL) at 0° C. was added in portions sodium borohydride (15.2 g, 0.4 mol). The mixture was stirred for 1 hour at room temperature, the solvent was azeotroped off with chloroform (5×300 mL). The residue was purified by silica gel chromatography with 10% methanol/90% dichloromethane/0.2% ammonium hydroxide to provide the title compound (15 g). MS (ESI) m/e 316 (M+H)+; 1H NMR (400 MHz, CD3OD) δ ppm 1.39 (m, 9 H) 2.35 (m, 1 H) 2.50 (m, 1 H) 2.72 (m, 2 H) 3.00 (m, 1 H) 3.13 (m, 2 H) 3.75 (m, 2 H) 3.94 (m, 1 H) 4.57 (m, 2 H).

Provenance & Evidence