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HRID 731969作成日:2026年10月26日

Water → 2-[4-(2,2-Dimethylbenzo[d]1,3-dioxolan-5-oxy)butoxy]-1,3-dichloro-5-(phenylmethoxy)benzene

https://huagongshe.com/reaction/731969

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Potassium CarbonateHCID 11430—
反応物Bendiocarb phenolHCID 62765—
反応物1,3-Dichloro-2-(4-chlorobutoxy)-5-(phenylmethoxy)benzeneHCID 22257123—
溶媒DimethylformamideHCID 6228—
生成物2-[4-(2,2-Dimethylbenzo[d]1,3-dioxolan-5-oxy)butoxy]-1,3-dichloro-5-(phenylmethoxy)benzeneHCID 6899988671.4%

反応手順

A stirred solution of 0.3 gram (0.00083 mole) of 1,3-dichloro-2-(4-chlorobutoxy)-5-(phenylmethoxy)benzene, 0.17 gram (0.00100 mole) of 2,2-dimethylbenzo[d]1,3-dioxolan-4-ol, and 0.17 gram (0.00125 mole) of potassium carbonate in 10 mL of DMF was heated at 80° C. for about 18 hours. After this time, the reaction mixture was cooled and 30 mL of water was added. The mixture was then extracted with three 20 mL portions of diethyl ether. The combined extracts were washed with 20 mL of an aqueous solution saturated with sodium chloride. The organic layer was dried with sodium sulfate, filtered, and concentrated under reduced pressure to a residue. The residue was purified with column chromatography on silica gel using 1:1 methylene chloride:hexane as an eluant. The appropriate fractions were combined and concentrated under reduced pressure, yielding 0.29 gram 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-59a35a2f9bb440a88ac7a187a0b59c5c
出典メモuspto-grants-2009_09