HuagongsheHuagongshe Chemistry Print Report · For research reference only
1H-1,2,4-Triazole → HCID 10113408, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1H-1,2,4-Triazole | HCID 9257 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22250442 | HCID 22250442 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10113408 | HCID 10113408 | 87% |
Reaction Steps
To a stirred solution of 1,2,4-triazol (105 mg, 1.52 mmol) in DMF (15 ml) was added at 0° C. sodium hydride (61 mg, 1.52 mmol; 60%-disp.). The mixture was stirred at RT for 1 h, cooled to 0° C. and (2RS,5RS)-2-(3-chloro-propyl)-5-(4-fluoro-phenyl)-1-(toluene-4-sulfonyl)-pyrrolidine (0.50 g, 1.26 mmol) was added. The reaction mixture was stirred at RT for 3 h and at 50° C. for 16 h, poured into ice/water (70 ml) and extracted with dichloromethane (2×100 ml). The combined organic layers were washed with water (70 ml) and brine (70 ml), dried (MgSO4) and evaporated. The crude product was purified by column chromatography on silica gel (ethyl acetate) to yield the title compound (0.47 g, yield 87%) as a colorless oil, MS: m/e=429.5 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06995182B2 |
| Source dataset | uspto-grants-2006_02 |
| ORD ID | ord-effd577ba14540d28ed6c5e02af6c590 |
| Source note | uspto-grants-2006_02 |