HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → HCID 58261502, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Reactant | Fluoranthen-3-ylboronic acid | HCID 23088535 | — |
| Reactant | HCID 58261495 | HCID 58261495 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58261502 | HCID 58261502 | — |
Reaction Steps
15.4 g (40 mmol) of diethyl 2-chloro-5-naphthalen-1-ylterephthalate, 14.0 g (56 mmol) of fluoranthene-3-boronic acid and 17.7 g of Cs2CO3 are initially introduced in 70 ml of dry dioxane and saturated with N2 for 30 min. 0.8 ml of a 1.0 M solution of tri-tert-butylphosphine in toluene, followed by 91 mg (0.4 mmol) of Pd(OAc)2 are then added. The mixture is heated at the boil for 4 h, extended with water and EtOH, the precipitate is filtered off with suction, washed with heptane and dried. The solid is recrystallised from toluene and then has, according to 1H-NMR, a purity of >95%. The yield is 8.5 g (38%) of colourless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051233B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-8a5f3191c8874fda8687ed65e553ef54 |
| Source note | uspto-grants-2015_06 |