Bromocyclopentane → HCID 19025756, compound

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Reaction Steps

0.6 g (80 % pure) of sodium hydride (0.02 mol) is suspended in 40 ml of absolute DMF at 0° C., and 5.5 g (0.02 mol) of the compound from Example I in 20 ml of DMF are added dropwise. Evolution of hydrogen starts. During this process, the temperature rises to room temperature. The mixture is subsequently stirred at room temperature for a further hour and then cooled to 0° C., and 3 g (0.02 mol) of cyclopentyl bromide are added dropwise. The mixture is allowed to react further overnight and then concentrated to dryness in vacuo, and the residue is extracted by stirring with 180 ml of water/methylene chloride (1: 1) . The organic phase is separated off, dried and concentrated to a small volume, and the residue is separated by column chromatography (silica gel 60, mobile phase: toluene/ethyl acetate 9:1).

Provenance & Evidence