Ethyl Acetate → HCID 77750102, compound

Participants

Reaction Conditions

Reaction Steps

DIBAL-H® (1.5M solution in toluene, 20 ml) was added to an ice-cooled solution of the product of Example 11, step a) (2.00 g) in toluene (30 ml) and the solution stirred at this temperature for 30 minutes before adding ethyl acetate (2 ml). The solution was washed with water and concentrated. The residue (1.8 g) was taken into ethanol and cooled to 4° C. before adding 3-chloroperoxybenzoic acid (50-55%, 2.5 g) and allowing the reaction to stir at room temperature for 18 hours. The solution was washed with aqueous sodium metabisulfite solution (3×10 ml) then dried and concentrated. Purification (SiO2, ether:isohexane, 80:20, as eluent) afforded the subtitle compound (1.8 g).

Provenance & Evidence