Hydrochloric Acid → HCID 23336680, compound

Participants

Reaction Steps

The product of step (f) (7.5 g) and diethyl oxalate (24.4 mls) in dry dimethylformamide (200 mls) were added to ether washed 50% sodium hydride (4.3 g) in dry dimethylformamide (250 mls) with stirring under nitrogen. The whole was stirred for a further 24 hours after addition, then poured into ice/water and extracted into ethyl acetate which was dried, filtered and the solvent evaporated to afford a red solid. This was added to ethanol (100 mls) previously saturated with hydrogen chloride gas and refluxed for 15 minutes. The reaction mixture was poured into water, extracted with chloroform, dried and the solvent evaporated to give 4.9 g of the desired product. Structure confirmed by MS and NMR.

Provenance & Evidence