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HRID 22629作成日:2026年10月26日

Hexane → Phenanthrene

https://huagongshe.com/reaction/22629

反応式

関与物質

役割名称HCID仕込み量
反応物HexaneHCID 8058—
反応物Ethyl AcetateHCID 8857—
反応物Dimethyl acetylenedicarboxylateHCID 12980—
反応物HCID 22056732HCID 22056732—
溶媒NitrobenzeneHCID 7416—
生成物PhenanthreneHCID 99561.2%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US06849367B2
出典データセットuspto-grants-2005_02
ORD IDord-966873ba36774f7eb74c09b8155b13af
出典メモuspto-grants-2005_02