HCID 58672952, compound → HCID 58672950, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of methyltriphenylphosphonium bromide (1.55 g, 4.34 mmol) in dry THF (10 mL) cooled to 0° C. was added n-butyl lithium (n-BuLi, 2.71 mL, 4.34 mmol, 1.6 M solution in hexane), and the mixture was stirred for 10 min, and further stirred for 1 h at room temperature. To the resulting orange mixture was added over ca. 20 min period a solution of Compound 6 (1.0 g, 2.15 mmol) dissolved in dry THF (10 mL). After being stirred for 1 h at 0° C. and for 17 h at room temperature, the reaction mixture was poured into ice water, and extracted with AcOEt. The organic layer was rinsed with saturated brine, and dried over anhydrous MgSO4. The solvent was removed by evaporation. The residue was purified by silica gel column chromatography (5 g; 2% AcOEt/hexane), to yield Compound 7 (978.5 mg, 98%, single compound).

Provenance & Evidence