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HRID 49526作成日:2026年10月25日

Dimethylformamide → 5-cyanomethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

https://huagongshe.com/reaction/49526

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Diethyl cyanophosphonateHCID 76257—
反応物4-(Trifluoromethyl)benzylamineHCID 76804—
反応物5-Cyanomethyl-2-methoxybenzoic acidHCID 17830574—
溶媒WaterHCID 962—
溶媒TriethylamineHCID 8471—
生成物5-cyanomethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamideHCID 17830578—

反応手順

To 2.55 g of publicly known 5-cyanomethyl-2-methoxybenzoic acid were added 50 ml of dimethylformamide, 2.57 g of 4-trifluoromethylbenzylamine, 2.66 g of diethyl cyanophosphonate and 2.00 ml of triethylamine, and the mixture was stirred for 20 minutes under cooling with ice and for 6 hours at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate. After washed with water, then with saturated brine, the organic layer was dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue was crystallized from hexane-diethyl ether and collected by filtration to obtain 4.44 g of 5-cyanomethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as colorless crystals. Melting point 124-125° C. Elemental analysis (%) C16H15F3N2O2 Calcd.(%) C, 62.07; H, 4.34; N, 8.04 Found (%) C, 62.03; H, 4.27; N, 7.99

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06706763B1
出典データセットuspto-grants-2004_03
ORD IDord-15fc2dc155604716b508d487d80a25d1
出典メモuspto-grants-2004_03