Water → HCID 68717205, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of 2.4 g (11.0 mmol) of phosphorous pentachloride in 7.0 mL of CH2Cl2 was added a solution of 2.28 g (9.0 mmol) of the product of Step A in 5.0 mL of CH2Cl2. The reaction mixture became homogenous while it was stiffed at room temperature for 3 h. The reaction mixture was then cooled to 0° C. with an external ice-water bath and ice and water were added. The reaction mixture was allowed to warm to room temperature while stirring for 1 h, and was then extracted with CH2Cl2. The organic layers were combined, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 5-20% EtOAc-hexane. Evaporation of the purified fractions afforded the title compound as a colorless oil.

Provenance & Evidence