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HRID 603349作成日:2026年10月24日

Potassium Carbonate → N-(2',6'-dichloro-4'-methylphenyl)-4-methylaniline

https://huagongshe.com/ja/reaction/603349

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2,6-Dichloro-4-methylphenolHCID 17077—
反応物2-Chloro-N-(4-methylphenyl)acetamideHCID 27967—
反応物Sodium MethoxideHCID 10942334—
反応物2-(2',6'-dichloro-4'-methylphenoxy)-N-(4-methylphenyl)acetamideHCID 57952155—
溶媒MethanolHCID 887—
溶媒IsopropanolHCID 3776—
溶媒HeptaneHCID 8900—
生成物N-(2',6'-dichloro-4'-methylphenyl)-4-methylanilineHCID 11369120—

反応条件

温度85 °C

反応手順

12 g (67 mmol) of 2,6-dichloro-4-methylphenol are dissolved in 25 ml of 2-propanol followed by the addition of 10.5 g (76 mmol) of potassium carbonate and 12.8 g (70 mmol) of 2-chloro-N-(4-methylphenyl)acetamide. The mixture is refluxed for 4 h. At this time, the formation of A: 2-(2′,6′-dichloro-4′-methylphenoxy)-N-(4-methylphenyl)acetamide is completed. 13.6 ml of sodium methylate solution 30% in methanol are slowly added and the temperature is increased to about 85° C. by distilling 25 ml of solvent. The mixture is stirred 2 h more to complete the formation of B. 25 ml of water are added at 70° C. to obtain a 2 phases solution. The lower layer is discarded. The upper layer is diluted with 20 ml of heptane-fraction and washed with 2×20 ml of water. The organic phase is separated and concentrated in vacuo to obtain N-(2′,6′-dichloro-4′-methylphenyl)-4-methylaniline as a crude oil. GC/MS: 265 (100, M+), 195 (130).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07906677B2
出典データセットuspto-grants-2011_03
ORD IDord-0161b63b7b774b7187cb7b9c172fc709
出典メモuspto-grants-2011_03