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HRID 643676作成日:2026年10月25日

Water → HCID 59261367、化合物

https://huagongshe.com/reaction/643676

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Potassium CarbonateHCID 11430—
反応物(e)-(2-Chlorobenzylidene)hydrazineHCID 9629214—
反応物2,4-Dichloro-6-methylpyridineHCID 11959083—
触媒CID 53485975HCID 53485975—
溶媒TolueneHCID 1140—
生成物HCID 59261367HCID 5926136731.4%

反応条件

温度100 °C

反応手順

(E)-1-(2-chlorobenzylidene)hydrazine (0.351 g, 2.27 mmol), dichloro[1,1′bis(diphenylphosphino)ferrocene]palladium (II) dichloromethane adduct (0.0185 g, 0.0227 mmol) and potassium carbonate (0.471 g, 3.41 mmol) was added to a 50-mL RBF. Toluene (2 mL) was added and 2,4-dichloro-6-methylpyridine (0.368 g, 2.27 mmol) in 3 mL of toluene was added. The red mixture was heated to 100° C. After 18 h, the reaction was allowed to cool to RT and water (20 mL) was added. The mixture was filtered and 190 mg of (E)-1-(2-chlorobenzylidene)-2-(4-chloro-6-methylpyridin-2-yl) hydrazine was collected as a tan solid. The filtrate was absorbed on silica gel and purified by silica gel chromatography (8/2 hexanes/DCM to 7/2/1 hexans/DCM/EtOAc) to afford an additional 200 mg of (E)-1-(2-chlorobenzylidene)-2-(4-chloro-6-methylpyridin-2-yl) hydrazine as a tan solid. MS (ESI, pos. ion) m/z: 280.0 (M+1).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07700593B2
出典データセットuspto-grants-2010_04
ORD IDord-18f87604d6eb4ec6913459692f7693df
出典メモuspto-grants-2010_04