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HRID 1098749作成日:2026年10月25日

Triethylamine → N-[1-(3-Pentafluoroethyl-phenyl)-vinyl]-acetamide

https://huagongshe.com/reaction/1098749

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物N-VinylacetamideHCID 78875—
反応物Phosphine, (1-methylethylidene)bis[diphenyl-HCID 12091099—
反応物Trifluoro-methanesulfonic acid 3-pentafluoroethyl-phenyl esterHCID 59506217—
触媒palladium(II) acetateHCID 167845—
溶媒DimethylformamideHCID 6228—
生成物N-[1-(3-Pentafluoroethyl-phenyl)-vinyl]-acetamideHCID 59506293—

反応条件

温度130 °C

反応手順

To a solution of the crude product of step 1 (0.75 g, 2.2 mmol) in DMF (10 ml) was added N-vinylacetamide (0.37 g, 4.36 mmol), triethylamine (243 mg, 0.33 ml, 2.40 mmol), palladium acetate (20 mg, 4 mol %) and bis(diphenylphosphino)propane (40 mg, 0.1 mmol). The reaction mixture was heated for 30 min at 130° C. using microwaves. The red solution was diluted and washed with hydrochloric acid (1M, 2×15 ml) and sodium hydrogen carbonate (saturated, 20 ml). The organic phase was dried over sodium sulphate and evaporated. Purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane (2:1) gave the desired product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08143242B2
出典データセットuspto-grants-2012_03
ORD IDord-952ca0b47f1a49ef9fa38068bfe476a6
出典メモuspto-grants-2012_03