Sodium Iodide → HCID 14882717, compound

Participants

Reaction Steps

A solution of 6.2 g of ethyl acetoacetate is added at 0° C. to a suspension of 1.13 g of sodium hydride in 150 ml of tetrahydrofuran. After 15 minutes at this temperature, 7.1 g of anhydrous sodium iodide are added, followed by the addition at 0° C. of l3.5g of the product obtained in Stage B. The mixture is then brought to reflux for 12 hours and the whole is thereafter concentrated, the residue is taken up in water and the product is extracted with dichloromethane. The 16.9 g of oil obtained are purified by chromatography on 900 g of silica (70-230 mesh), using a mixture of dichloromethane and methanol (98:2 V/V) as eluant.

Provenance & Evidence