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HRID 1023作成日:2026年10月23日

Acetic Acid → HCID 178418358、化合物

https://huagongshe.com/ja/reaction/1023

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物1,1-DichloroethaneHCID 6365—
反応物Ethyl orthoformateHCID 31214—
反応物4-PhenylcyclohexanoneHCID 78605—
反応物Sodium BicarbonateHCID 516892—
反応物Sodium triacetoxyborohydrideHCID 5049666—
反応物3-Bromo-2-ethylpyridin-4-amineHCID 54573798—
触媒Boron trifluoride etherateHCID 8000—
溶媒EthanolHCID 702—
生成物HCID 178418358HCID 178418358—

反応条件

温度50 °C

反応手順

3.48 g (20 mmol) of 4-phenylcyclohexanone in 3.3 ml of ethanol are treated with 3.3 ml of triethyl orthoformate and 2 drops of boron trifluoride etherate and warmed at 50° C. for 30 min. After addition of 2.01 g (10mmol) of 2-ethyl-3-bromo-4-aminopyridine the reaction mixture is heated at 135°-140° C. for 3.5-4 hours with simultaneous removal of the low-boiling components by distillation. It is then cooled, 40 ml of dichloroethane, 3.18 g (15 mmol) of sodium triacetoxyborohydride and 0.57 ml (10 mmol) of glacial acetic acid are added, and it is heated at 50°-60° C. for 3 hours; the reaction mixture is then cooled, saturated aqueous sodium hydrogen carbonate solution is added, the 1,2-dichloroethane is evaporated and the reaction product is extracted from the aqueous phase using ethyl acetate. Purification is carried out by column chromatography. Yield: 1.46 g (41%); RF =0.59 (ethyl acetate)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05723450
出典データセットuspto-grants-1998_03
ORD IDord-5d3b4c5598fc43c8868c332153f62858
出典メモuspto-grants-1998_03