HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 15986279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Tributylvinyltin | HCID 81998 | — |
| Reactant | HCID 49830947 | HCID 49830947 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 15986279 | HCID 15986279 | 33% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 2-chloro-5,10-dihydro-3,4,5,10-tetraaza-dibenzo[a,d]cyclohepten-11-one from Example 2 (150 mg, 0.61 mmol) in toluene (3 ml) was added tri-n-butyl(vinyl)tin (231 mg, 0.73 mmol) followed by triphenylphosphine (4.8 mg, 0.02 mmol) and tetrakistriphenylphosphine palladium (7 mg, 0.01 mmol) and the resulting mixture was heated at 100° C. for 15 hours. The mixture was cooled to room temperature, concentrated in vacuo and purified directly by flash column chromatography (silica gel, 10% MeOH 90% dichloromethane) to afford the title compound as a yellow solid (47 mg, 33%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994160B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-5a0a7474e8d8429e98b6818c83e7e0c6 |
| Source note | uspto-grants-2011_08 |