Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 19773344 | HCID 19773344 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19773289 | HCID 19773289 | — |
Reaction Steps
0.48 g (0.0015 mol) of 5-(N-acetyl-N-propargyl-amino)-2-n-propylamino-tetraline-hydrochloride (Example 4.7.11) are refluxed in 10 ml of ethanol and 30 ml of 6 N hydrochloric acid for 16 hours. The mixture is then concentrated by rotary evaporation, finally at 80° C. under a complete water-jet vacuum. The residue is shaken with 50 ml of water, 50 ml of methylene chloride and excess ammonia. The aqueous phase separated off is extracted twice more with 15 ml of methylene chloride. The combined methylene chloride extracts are washed with 20 ml of water and concentrated by rotary evaporation as described above. The residue is crystallised analogously to Example 4.1.1 in the form of the dihydrochloride. Yield 0.12 g (25.2% of theory), melting point 198° C., unchanged after recrystallisation from ethanol/ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05196454 |
|---|
| Source dataset | uspto-grants-1993_03 |
|---|
| ORD ID | ord-d486e7a2c7574cb8a026af3353029fa7 |
|---|
| Source note | uspto-grants-1993_03 |
|---|