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HRID 1374623作成日:2026年10月27日

Cesium carbonate → 6-[4-(2-Bromo-5-fluorophenyl)-2-hydroxy-4-methyl-2-trifluoromethylvaleroylamino]-4-methyl-2,3-benzoxazin-1-one

https://huagongshe.com/reaction/1374623

反応式

関与物質

役割名称HCID仕込み量
反応物Cesium carbonateHCID 10796—
反応物SilaneHCID 23953—
反応物(Trifluoromethyl)trimethylsilaneHCID 552549—
反応物6-[4-(2-Bromo-5-fluorophenyl)-4-methyl-2-oxovaleroylamino]-4-methyl-2,3-benzoxazin-1-oneHCID 21908380—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物6-[4-(2-Bromo-5-fluorophenyl)-2-hydroxy-4-methyl-2-trifluoromethylvaleroylamino]-4-methyl-2,3-benzoxazin-1-oneHCID 2190830668.7%

反応手順

0.23 ml (1.25 mmol) of trifluoromethyl(trimethyl)silane and 256 mg (0.79 mmol) of cesium carbonate are added at 0° C. to a solution of 290 mg (0.63 mmol) of 6-[4-(2-bromo-5-fluorophenyl)-4-methyl-2-oxovaleroylamino]-4-methyl-2,3-benzoxazin-1-one in 7 ml of DMF. After 24 hours, the same amount of silane and base are added and stirred for another 24 hours at room temperature. The batch is diluted with 150 ml of ethyl acetate, washed with water and saturated NaCl, dried (Na2SO4) and concentrated by evaporation in a vacuum. Purification by column chromatography of the residue on silica gel yields 230 mg of product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07166592B2
出典データセットuspto-grants-2007_01
ORD IDord-0308a47e6c3442bca614be210a71472d
出典メモuspto-grants-2007_01