Ethane, 1-fluoro-2-iodo- → HCID 86653735, compound

Participants

Reaction Conditions

Reaction Steps

In a sealed tube, 0.53 g of NaHCO3 (6.4 mmol) and 0.49 g of 1-iodo-2-fluoroethane (2.8 mmol) are added to 0.88 g (2.6 mmol) of the compound obtained from step 1.10 dissolved in DMF (6 ml). The sealed tube is heated at 90° C. for 5 hours. The reaction mixture is cooled, the DMF is then evaporated off under reduced pressure, and the residue obtained is taken up in water (10 ml) and extracted with ethyl acetate (20 ml×2). The organic phase is dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue obtained is purified by flash chromatography on silica gel (eluent: dichloromethane/methanol, 1% NH4OH), with a gradient of 0% to 10% methanol. 0.82 g of compound is obtained, in the form of a beige-coloured powder. Yield=85%. Melting point: 96° C. MH+: 391 (tr: 5.1 min., condition 1)

Provenance & Evidence