Triethylamine → HCID 9834346, compound

Temperature

20 °C

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).

1. customthe solvent is then largely removed on a rotary evaporator
2. washthe mixture is washed with 1N NaOH solution
3. customthe organic phase is dried
4. customthe solvent is removed by distillation on a rotary evaporator
5. customIn order to remove impurities of the bis-acylated compound
6. temperaturethe mixture is warmed at 50° C. with 200 ml of 1N sodium hydroxide solution for one hour
7. customIt is evaporated on a rotary evaporator again
8. extractionthe residue is extracted with CH2Cl2 /H2O
9. customthe organic phase is dried
10. customevaporated on a rotary evaporator
11. distillationthe residue is distilled in a bulb tube oven (boiling point0.2 =165° C)

ORD record

ord-263cc2598e844704a08f40ad7e87014c

Source dataset

uspto-grants-1989_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04873252