Oxalic Acid → HCID 77750336, compound

Participants

Reaction Steps

A solution of the product of Example 1, step (a) (1.6 g) in dimethylsulphoxide (15 ml) was treated with pyridine (0.25 g) followed by trifluoroacetic acid (0.18 g). To this mixture was added 1,3-dicyclohexylcarbodiimide (1.99 g). After stirring for 5 hours at the reaction mixture was treated with methyl(triphenylphosphoranylidene)acetate (1.72 g) and then stirred for a further 18 hours. The mixture was poured into ethyl acetate (300 ml) and treated with oxalic acid (1.59 g). After stirring for 30 minutes the mixture was filtered and the ethyl acetate solution was washed with dilute aqueous sodium bicarbonate and then with dilute aqueous brine, before being dried and concentrated. Purification (SiO2, ethyl acetate:isohexane 1:4 as eluant) afforded the subtitle compound (1.5 g).

Provenance & Evidence