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HRID 366296作成日:2026年10月25日

Triphenylphosphine → (E)-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(4,4,4-trifluorobut-2-enyloxy)pyridine

https://huagongshe.com/reaction/366296

反応式

関与物質

役割名称HCID仕込み量
反応物TriphenylphosphineHCID 11776—
反応物ethyl N-ethoxycarbonyliminocarbamateHCID 220568—
反応物4,4,4-Trifluoro-2-buten-1-olHCID 2777076—
反応物HCID 178429419HCID 178429419—
溶媒1,4-DioxaneHCID 31275—
溶媒Ethyl acetate pentaneHCID 22335286—
生成物(E)-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(4,4,4-trifluorobut-2-enyloxy)pyridineHCID 1547717399.4%

反応手順

A mixture of 6-hydroxy-2-(l-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (0.8 g, 2.93 mmol), 4,4,4-trifluorobut-2-en-1-ol (0.44 g, 3.5 mmol), triphenylphosphine (0.92 g, 3.51 mmol) and diethyl azodicarboxylate (0.61 g, 3.51 mmol) in dry dioxane (3 ml) is stirred for 1.5 h at ambient temperature. The reaction mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (1.11 g, 70 % yield) as an colorless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06130188
出典データセットuspto-grants-2000_10
ORD IDord-815afd78947a4d5985e4c7d30e02566d
出典メモuspto-grants-2000_10