Dimethylamine → HCID 12664027, compound

To 1000 g of Klinosorb-4 molecular sieve 500 ml of dry ether and 226 g of 1-methyl-4-piperidone are added and thereafter dimethylamine gas is bubbled into the reaction mixture with a rate allowing only slow reflux of the mixture in the initial period of the reaction. The dimethylamine gas is introduced into the reaction medium for 8 hours on three subsequent days, thereafter the mixture is filtered, the Klinosorb is washed with ether and the combined etheral solution is evaporated to dryness under reduced pressure. The oily residue is purified by distillation in vacum to yield 70% of 1-methyl-4-dimethylamino-1,2,5,6-tetrahydropyridine; bp.: 78°-82° C./2.66 kPa.

1. customdimethylamine gas is bubbled into the reaction mixture with a rate
2. temperatureallowing only slow reflux of the mixture in the initial
3. customperiod of the reaction
4. filtrationthe mixture is filtered
5. washthe Klinosorb is washed with ether
6. customthe combined etheral solution is evaporated to dryness under reduced pressure
7. distillationThe oily residue is purified by distillation in vacum

ORD record

ord-5687dc2461aa4f209351c71ac4c01fab

Source dataset

uspto-grants-1988_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04769373