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Hexane → Phenanthrene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Dimethyl acetylenedicarboxylate | HCID 12980 | — |
| 反応物 | HCID 22056732 | HCID 22056732 | — |
| 溶媒 | Nitrobenzene | HCID 7416 | — |
| 生成物 | Phenanthrene | HCID 995 | 61.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849367B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-966873ba36774f7eb74c09b8155b13af |
| 出典メモ | uspto-grants-2005_02 |