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HRID 460029作成日:2026年10月26日

Ethanol → HCID 86592488、化合物

https://huagongshe.com/reaction/460029

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物Sodium hydrideHCID 24758—
反応物4-Methyl-2-[4-(trifluoromethyl)phenyl]-1,3-thiazole-5-carbaldehydeHCID 2782899—
反応物HCID 16109177HCID 16109177—
溶媒WaterHCID 962—
生成物HCID 86592488HCID 86592488—

反応手順

Sodium hydride (0.040 g, 60% dispersion in mineral oil) was added to anhydrous ethanol (20 ml) followed by [4-(2-ethoxy-2-oxoethoxy)-3-methylbenzyl](triphenyl)phosphonium chloride (intermediate 18, 0.45 g) after 10 minutes. After a further 10 minutes 4-methyl-2-[4-(trifluoromethyl)phenyl]-1,3-thiazole-5-carbaldehyde (intermediate 2, 0.24 g) was added and the reaction mixture stirred at ambient temperature for 3 hours. The reaction mixture was treated with water and then the mixture extracted with chloroform. The chloroform solution was separated with a hydrophobic frit and excess aldehyde removed using 3-[4-(hydrazinosulfonyl)phenyl]propionyl AM resin (0.50 g). The crude product remaining after this treatment was purified by Biotage™ chromatography using a mixture of petroleum ether:ethyl acetate (5:1) as eluent to give the title compound as a mixture of E and Z isomers.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07196107B2
出典データセットuspto-grants-2007_03
ORD IDord-9e71b5a9e3f240a0886e6c872cbe7695
出典メモuspto-grants-2007_03