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HRID 639720作成日:2026年10月26日

Dimethyl Sulfoxide → 3-[(2-Methoxyethoxy)carbonylamino]benzaldehyde

https://huagongshe.com/reaction/639720

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl SulfoxideHCID 679—
反応物TriethylamineHCID 8471—
反応物Oxalyl chlorideHCID 65578—
反応物HCID 67347770HCID 67347770—
溶媒WaterHCID 962—
溶媒DichloromethaneHCID 6344—
生成物3-[(2-Methoxyethoxy)carbonylamino]benzaldehydeHCID 2313180658.6%

反応条件

温度-60 °C

反応手順

To a mixture of 13 ml of oxalyl chloride and 400 ml of dichloromethane was added dropwise a solution of 23 ml of dimethyl sulfoxide in 40 ml of dichloromethane at −60° C. for 15 minutes. After stirred at −60° C. for 10 minutes, a solution of 30.2 g of 3-[(2-methoxyethoxy)carbonylamino]benzyl alcohol in 100 ml of dichloromethane was added dropwise at −60° C. for 25 minutes. After stirred at −60° C. for 20 minutes, 56 ml of triethylamine was added dropwise at −60° C. for 15 minutes. After stirred at room temperature for 45 minutes, water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer washed successively with water and then an aqueous saturated sodium chloride solution. After dried over anhydrous magnesium sulfate and then concentration, the resulting crude crystals were washed with t-butyl methyl ether and then dried to obtain 17.55 g of 3-[(2-methoxyethoxy)carbonylamino]benzaldehyde [Compound No. (h)] as a white solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07691883B2
出典データセットuspto-grants-2010_04
ORD IDord-3a24fcfa20a745978525ddc26b73f1b8
出典メモuspto-grants-2010_04