Hexane → HCID 86743747, compound

Participants

Reaction Steps

At 0° to 5° C., 87.5 ml of 1.6 molar BuLi solution in hexan (0.14 mol) are added dropwise to 23 g (0.13 mol) of methanesulphonic acid-N'-methylpiperazide dissolved in 200 ml of anhydrous tetrahydrofuran, the resulting suspension is stirred for 90 minutes at ambient temperature and then 23.4 g of 2-(2-bromoethyl)-1,3-dioxolan (0.13 mol) in 200 ml of anhydrous tetrahydrofuran are added dropwise, forming a clear solution. After 5 hours' stirring the solvent is eliminated, the residue is taken up with water/methylene chloride and the aqueous phase is extracted several times with methylene chloride. The methylene chloride solution is dried and the solvent is drawn off. The oil residue is filtered over a column of silica gel using methylene chloride/methanol 9:1 as eluant. After the solvent has been driven off again, 20.7 of the desired compound are obtained as a light coloured oil.

Provenance & Evidence