HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67195867, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86669224 | HCID 86669224 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67195867 | HCID 67195867 | 70% |
Reaction Steps
To a suspension of {(cis)-1-acetyl-2-methyl-6-[4-(1-piperidinylmethyl)phenyl]-1,2,3,4-tetrahydro-4-quinolinyl}formamide (for a preparation see Intermediate 30) (109 g, 0.27 mol) in MeOH (1 L) was added 6N HCl (136 mL, 0.8 mol). The resulting homogenous mixture was stirred at reflux for 2 hours and concentrated under vacuo. The residue was taken up in water (1 L) and washed with DCM (100 mL). The aqueous phase was basified with NaHCO3 and the organic materials were extracted with DCM (2×0.5 L) dried over Na2SO4 and concentrated to dryness. After heating of the residue in DCM (100 mL) and iPr2O (1 L) and filtration the title compound was obtained as a white precipitate (70 g, 70%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697725B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-4a2a0cc46d3346039e955a635560e91b |
| Source note | uspto-grants-2014_04 |