Triethylamine → HCID 178461109, Verbindung

0.220 g (2.2 mmol) Triethylamine, a spatula tip of tetrabutylammonium iodide and 0.340 g (2.2 mmol) of cis-4-tert-butylcyclohexylamine were added successively to a solution of 0.470 g (2.0 mmol) of 5-(1-fluoroethyl)-6,7-dichloro-[1,2,4]triazolo[1,5-a]pyrimidine in 15 ml of toluene under stirring. The reaction mixture was heated at reflux for 5 hours and then stirred for another 12 hours at room temperature. The solvent was evaporated under reduced pressure and dichloromethane was added to the resulting residue. The resulting reaction mixture was washed with 2N hydrochloric acid and water. The organic phase was separated, dried and the solvent was evaporated under reduced pressure. Treatment of the resulting residue with hexane yielded 0.540 g (1.5 mmol, 76% of theory) of the title compound having a melting point of 138-139° C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 5 hours
3. stirringstirred for another 12 hours at room temperature
4. customThe solvent was evaporated under reduced pressure and dichloromethane
5. additionwas added to the resulting residue
6. customThe resulting reaction mixture
7. washwas washed with 2N hydrochloric acid and water
8. customThe organic phase was separated
9. customdried
10. customthe solvent was evaporated under reduced pressure

ORD-Eintrag

ord-b3856b4e115446bdb110b713d9e0fb18

Quelldatensatz

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08664235B2