HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexachloroethane → HCID 86686960, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 86686959 | HCID 86686959 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86686960 | HCID 86686960 | 82.2% |
Reaction Steps
Hexachloroethane (1.77 g, 7.75 mmol) was added portionwise to a solution of Intermediate 8a 822 mg, 3.87 mmol), triphenylphosphine (2.03 g, 7.75 mmol) and triethylamine (2.2 mL, 15.49 mmol) in dry THF (15 mL) at RT and stirred for 16 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 a buff-coloured foam (618 mg, 82%). LCMS (Method 1): Rt 1.55 min, m/z 195 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08907094B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-191f7f5aeaa5470cb0831913aaf1705c |
| Source note | uspto-grants-2014_12 |