HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59850164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Stannous Chloride | HCID 24479 | — |
| Reactant | HCID 59850146 | HCID 59850146 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59850164 | HCID 59850164 | 97.1% |
Reaction Steps
A stirred mixture of N-(5-cyclopropyl-4-fluoro-2-nitrophenyl)-1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine (D81, 0.38 g, 1.05 mmol), tin (II) chloride (0.8 mg, 4.20 mmol) and conc. HCl acid (˜0.9 ml) in abs ethanol (30 ml) was heated at gentle reflux temperature for 18 hrs. After cooling, the majority of solvent was removed by concentration under reduced pressure and the residue treated with dilute K2CO3 solution (50 ml) and extracted with ethyl acetate, filtering the mixture to remove tin residues. The separated organic phase was dried (MgSO4) and concentrated to dryness under vacuum to afford the title compound as a pale brown oil (340 mg, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288412B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-ff3b20d8697e4a93aa63e8dd3dae8836 |
| Source note | uspto-grants-2012_10 |