HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromobenzene → HCID 66797829, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromobenzene | HCID 7961 | — |
| Reactant | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 66797653 | HCID 66797653 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | P-Xylene | HCID 7809 | — |
| Product | HCID 66797829 | HCID 66797829 | — |
Reaction Steps
21.0 g (26 mmol) of 7-{10-(4,6-diphenyl-1,3,5-triazin-2-yl)-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorenyl}-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene, 2.8 g (27 mmol) of bromobenzene and 6.8 g (71 mmol) of NaOtBu are suspended in 1000 ml of p-xylene. 0.11 g (0.5 mmol) of Pd(OAc)2 and 0.33 ml of a 1 M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 16 h. After cooling, the organic phase is separated off, washed three times with 100 ml of water and subsequently evaporated to dryness. The residue is extracted with hot toluene, recrystallised from toluene and finally sublimed in a high vacuum. The yield is 15.3 g (18 mmol, 66.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126970B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-5a70fffef43d405682eb080f2b2cef42 |
| Source note | uspto-grants-2015_09 |