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HRID 731967作成日:2026年10月26日

Pyrogallol → Bendiocarb phenol

https://huagongshe.com/reaction/731967

反応式

関与物質

役割名称HCID仕込み量
反応物PyrogallolHCID 1057—
反応物2,2-DimethoxypropaneHCID 6495—
溶媒TolueneHCID 1140—
生成物Bendiocarb phenolHCID 6276540.4%

反応手順

A stirred mixture of 10.0 grams (0.079 mole) of benzene-1,2,3-triol, 20 mL (0.163 mole) of 2,2-dimethoxypropane and 1.0 gram (catalyst) of Amberlite® IR-120 (plus) ion exchange resin in 50 mL of toluene was warmed to 100° C., where it was maintained during an 18 hour period. After this time the reaction mixture was concentrated under reduced pressure to a residual solid. The solid was triturated with three 50 mL portions of methylene chloride. The combined organic extracts were concentrated under reduced pressure to a residual solid, which was then dissolved in methylene chloride and subjected to column chromatography on silical gel. Elution was accomplished with 1:4 ethyl acetate:hexane. A second column chromatography as described above was needed to purify the solid. In each chromatography, the appropriate fractions were combined and concentrated under reduced pressure, ultimately yielding 5.3 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07585891B2
出典データセットuspto-grants-2009_09
ORD IDord-a47299d14d7f4261b3c3b3c0e9e19ed2
出典メモuspto-grants-2009_09