HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexachloroethane → HCID 86686951, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Piperidine-1-carboxylic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide | HCID 86686950 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86686951 | HCID 86686951 | 48% |
Reaction Steps
Hexachloroethane (826 mg, 3.92 mmol) was added portionwise to a solution of Intermediate 3a (466 mg, 1.95 mmol), triphenylphosphine (1.03 g, 3.92 mmol) and triethylamine (1.1 mL, 7.83 mmol) in dry THF (30 mL) at RT, and the mixture stirred for 2 h. The resulting precipitate was filtered off and the filtrate evaporated. The residue was purified by SCX-2, eluting with MeOH followed by 2M NH3 in MeOH, to give the title compound as pale orange coloured gum (206 mg, 48%). LCMS (Method 1): Rt 2.44 min, m/z 221 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09139584B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-a192c04974c34e8faf4026e821ff4db5 |
| Source note | uspto-grants-2015_09 |