HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 86213022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Dimethyl acetylenedicarboxylate | HCID 12980 | — |
| Reactant | 1-Ethenyl-4-methoxynaphthalene | HCID 22056732 | — |
| Solvent | Nitrobenzene | HCID 7416 | — |
| Product | HCID 86213022 | HCID 86213022 | 61.2% |
Reaction Steps
1-methoxy-4-vinyl naphthalene 18.42 g (0.1 mol) and acetylene dicarboxylic acid dimethyl ester 28.42 g (0.2 mol) were dissolved in nitrobenzene, 200 ml, and they were reacted for 7 hours at the temperature of 130° C. After cooling, nitrobenzene was escaped in vapor under a reduced pressure condition, silica gel column chromatography (developing solvent n-hexane:an acetic acid ethyl=9:1) process was performed to residual elements, crude material, 23.08 g, was obtained. Further, objective phenanthrene compounds, 19.85 g (yield 61.2%) was obtained by recrystallizing from n-butanol. A melting point was 150.2 to 151.0° C. An infrared absorption spectrum of this phenanthrene compound is shown in FIG. 4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07175958B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-9d186c56330844cb8b8f1f8d912bc6a3 |
| Source note | uspto-grants-2007_02 |