HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributyltin azide → HCID 178489540, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributyltin azide | HCID 4984872 | — |
| Reactant | HCID 68499085 | HCID 68499085 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178489540 | HCID 178489540 | — |
Reaction Steps
A solution of 0.40 g of tert-butyl 3-{2-[2-(3-cyanopropyl)phenoxy]ethoxy}-4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}piperidine-1-carboxylate (Example 55a) and 0.34 ml of tributyltin azide in 8 ml of o-xylene is stirred at 145° C. over 19 hours. The reaction mixture is concentrated by evaporation, the residue is taken up in 12.5 ml of 40:10:1 dichloromethane-methanol-25% conc. ammonia and stirred at room temperature over 1 hour. The mixture is concentrated by evaporation. The title compound is obtained as a yellow resin from the residue by means of flash chromatography (SiO2 60F). Rf=0.65 (40:10:1 dichloromethane-methanol-25% conc. ammonia); Rt=5.61.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07842688B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-e5e2a653385840afaafd9dbeec205ef4 |
| Source note | uspto-grants-2010_11 |