HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexachloroethane → HCID 86687117, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 86687118 | HCID 86687118 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86687117 | HCID 86687117 | 41.4% |
Reaction Steps
To a solution of Intermediate 85h (1.37 g, 2.08 mmol), Ph3P (1.09 g, 4.16 mmol) and Et3N (840 mg, 8.32 mmol) in THF (60 mL) was added hexachloroethane (980 mg, 4.16 mmol) and the mixture stirred at RT for 20 h. The mixture was diluted with DCM, washed with 10% aq. K2CO3 solution, brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by FCC, using 0-100% EtOAc in cyclohexane, to give the title compound as a clear oil (350 mg, 41%). LCMS (Method 4): Rt 3.07 min, m/z 407 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08907094B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-3b2ebf23df534fcc90c1e30b06864f21 |
| Source note | uspto-grants-2014_12 |