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HRID 967472作成日:2026年10月27日

Triphenylphosphine → 4-Chloro-3-[2-(2,4-dichloro-phenyl)-ethoxy]-benzoic Acid Methyl Ester

https://huagongshe.com/reaction/967472

反応式

関与物質

役割名称HCID仕込み量
反応物TriphenylphosphineHCID 11776—
反応物2,4-Dichlorophenethyl alcoholHCID 2734099—
反応物Diethyl azodicarboxylateHCID 5462977—
反応物Methyl 4-chloro-3-hydroxybenzoateHCID 11819787—
溶媒TetrahydrofuranHCID 8028—
生成物4-Chloro-3-[2-(2,4-dichloro-phenyl)-ethoxy]-benzoic Acid Methyl EsterHCID 69652287—

反応手順

2.0 g (10.72 mmol) of 4-Chloro-3-hydroxy-benzoic acid methyl ester was dissolved in 20 ml of anhydrous tetrahydrofuran. To this solution was added 2.25 g (11.79 mmol) of 2-(2,4-Dichlorophenyl)-ethanol, 10.71 g (equivalent to 32.2 mmol PPh3) of triphenylphosphine derivatized polystyrene and 5.6 g (32.2 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/6).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06953857B2
出典データセットuspto-grants-2005_10
ORD IDord-b316ee85efe943cba3f6ed291f32e5cb
出典メモuspto-grants-2005_10