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HRID 968437作成日:2026年10月24日

Potassium Carbonate → HCID 178517846、化合物

https://huagongshe.com/ja/reaction/968437

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物3-MorpholinoneHCID 66953—
反応物Ammonium cerium (IV) nitrateHCID 9869224—
反応物Ethyl acetate methanol diethylamineHCID 22289840—
溶媒WaterHCID 962—
溶媒AcetonitrileHCID 6342—
生成物HCID 178517846HCID 178517846—

反応条件

温度40 °C

反応手順

A mixture of the protected morpholinone of Preparation 53 (500 mg, 1.66 mmol), and ammonium cerium (IV) nitrate (2.5 g, 4.5 mmol) in water (6 ml) and acetonitrile (6 ml) was stirred at 40° C. for 18 hours. Potassium carbonate (1.5 g) was added and the mixture was stirred for 10 minutes then adsorbed onto silica gel. The product was isolated by column chromatography on silica gel using ethyl acetate:methanol:diethylamine (96:2:2 to 80:10:10) and was further purified by column chromatography on silica gel using dichloromethane:methanol (90:10 to 85:15) to afford the title compound, 240 mg. 1H-NMR (CD3OD, 400 MHz) δ: 3.02-3.42 (m, 4H), 3.78 (m, 1H0, 4.00 (m, 1H), 4.38 (m, 1H), 6.75 (s, 1H), 7.78 (s, 1H). HRMS: m/z (ES+) 182.0924 [MH+]

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06958402B2
出典データセットuspto-grants-2005_10
ORD IDord-f07fff6300404df58f97c65d192a3edb
出典メモuspto-grants-2005_10