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HRID 526700作成日:2026年10月26日

Diethyl Oxalate → Lithium 3-ethoxycarbonyl-2-methyl-3-oxo-1-(4-trifluoromethyl-phenyl)-propan-1-olate

https://huagongshe.com/reaction/526700

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl OxalateHCID 7268—
反応物p-TrifluoromethylpropiophenoneHCID 136554—
反応物Lithium HexamethyldisilazideHCID 2733832—
溶媒MethylcyclohexaneHCID 7962—
生成物Lithium 3-ethoxycarbonyl-2-methyl-3-oxo-1-(4-trifluoromethyl-phenyl)-propan-1-olateHCID 89907367—

反応手順

To a solution of 118 ml of lithium bis(trimethylsilyl)amide (Lithium Hexamethyldisilazide; 0.9 M in methylcyclohexane) was added dropwise over 15 min, 20 g of 1-(4-Trifluoromethyl-phenyl)-propan-1-one in 51 ml methylcyclohexane at while maintaining the reaction mixture at 15-25° C. After stirring for 2 h, 15 ml of diethyl oxalate were added dropwise over 30 min and the reaction mixture was stirred for 16 h. Then, the precipitated product was collected by filtration and washed with n-heptane. The isolated crude product was used in the next reaction step after drying in vacuo. Yield: 19 g.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09346762B2
出典データセットuspto-grants-2016_05
ORD IDord-4358440f53fd4cc690d9f70c1e95c80a
出典メモuspto-grants-2016_05