Ethyl Acetate → HCID 23679692, compound

Participants

Reaction Steps

The product from step 1 (26 mg, 0.043 mmol), triphenylphosphine (4.0 mg, 0.015 mmol), 0.5M sodium 2-ethyl-hexanoate in ethyl acetate (0.095 mL, 0.048 mmol), and 0.5M 2-ethyl-hexanoic acid in ethyl acetate (0.095 mL, 0.048 mmol) were dissolved in 1:1 dichloromethane-ethyl acetate (1.5 mL). Tetrakis(triphenylphosphine)palladium(0) (6 mg, 0.005 mmol) was added and the resulting mixture was stirred at room temperature for 15 minutes. The mixture was diluted with diethyl ether and extracted with water (2 mL). The aqueous extracts were purified by preparative layer chromatography on a 1 mm×20 cm×20 cm RPSF plate, using 3:1 water-acetonitrile as the developing solvent. The product band was located by UV, removed and eluted with 4:1 acetonitrile-water. The eluent was concentrated under vacuum to remove the acetonitrile and lyophilized to afford the title compound (9.7 mg) as an amorphous solid.

Provenance & Evidence