HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloride → HCID 86698846, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloride | HCID 312 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 66577920 | HCID 66577920 | — |
| Product | HCID 86698846 | HCID 86698846 | 35% |
Reaction Steps
To a suspension of activated Zn—Cu complex (1.4 g, 19 mmol) and 4-bromo-1-ethenyl-2-methoxybenzene (2.700 g, 12.67 mmol) in dry tetrahydrofuran (30 mL) was added dropwise through addition funnel a solution of thrichloroacetic chloride (2.11 g, 19.0 mmol) and phosphoryl chloride (11.7 ml, 12.7 mmol) in tetrahydrofuran (20 mL) during 2 hr at refluxing temperature. Then the mixture was stirred overnight under refluxing temperature. The mixture was cooled to room temperature and filtered. The filtrate was combined with ethyl acetate (100 mL), the combined solution was concentrated to give the title compound (1.45 g, 35%) which was used into next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889730B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-ced7499fdb8e4dca9262201d9773526b |
| Source note | uspto-grants-2014_11 |