Triethylamine → HCID 9834346, compound

Participants

Reaction Conditions

Reaction Steps

65 g (0.5 mol) of 2-(2-hydroxyethyl)-piperidine and 90 ml of triethylamine (0.64 mol) are dissolved in 1 liter of tetrahydrofuran, and 80 ml (0.67 mol) of valeryl chloride are added at -20° C. The mixture is warmed at 20° C. for one day and the solvent is then largely removed on a rotary evaporator; the residue is taken up in methylene chloride, the mixture is washed with 1N NaOH solution, the organic phase is dried and the solvent is removed by distillation on a rotary evaporator. In order to remove impurities of the bis-acylated compound, the product is taken up in 200 ml of ethanol and the mixture is warmed at 50° C. with 200 ml of 1N sodium hydroxide solution for one hour. It is evaporated on a rotary evaporator again, the residue is extracted with CH2Cl2 /H2O, the organic phase is dried and evaporated on a rotary evaporator and the residue is distilled in a bulb tube oven (boiling point0.2 =165° C).

Provenance & Evidence