HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophenol → HCID 67421842, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 67422163 | HCID 67422163 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67421842 | HCID 67421842 | 80% |
Reaction Steps
A mixture of 3,3′-dimethyl-1′-[1-(2-nitro-benzenesulfonyl)-azetidin-3-ylmethyl]-1′,2′,3′4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (168 mg, 0.322 mmol), thiophenol (0.3 mL), K2CO3 (500 mg) in CH3CN (5 mL) were stirred at room temperature for 17 hours. The volatiles were removed under reduced pressure and saturated NaHCO3 (15 mL) was added and the mixture was extracted with CH2Cl2 (3×30 mL). The combined organic extracts were dried (MgSO4), filtered and concentrated. The crude material was subjected to column chromatography on silica gel (10:1:0.1 CH2Cl2:CH3OH:NH4OH; then 10:1:0.5) to provide 1′-azetidin-3-ylmethyl-1′,2′,3′4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (74 mg, 80% pure by LC/MS).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501518B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-66f1a9641cb44e7daa1ddf8302288fe0 |
| Source note | uspto-grants-2009_03 |