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HRID 586130作成日:2026年10月27日

1,2-Dichloroethane → N-ethyl-N-4-methoxybenzyl 2,6-dihydroxybenzamide

https://huagongshe.com/reaction/586130

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物2,6-Dihydroxybenzoic AcidHCID 9338—
反応物HOAtHCID 181649—
反応物Benzenemethanamine, N-ethyl-4-methoxy-HCID 296018—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物N-ethyl-N-4-methoxybenzyl 2,6-dihydroxybenzamideHCID 2232860232.3%

反応手順

To a stirred solution of N-ethyl-4-methoxybenzyl amine (1.07 g, 6.49 mmol) in DMF (10 mL) was added 2,6-dihydroxybenzoic acid (1.0 g, 6.49 mmol) followed by HOAt (0.97 g, 7.14 mmol) and EDC (1.31 g, 6.81 mmol). After stirring overnight, the reaction was diluted with EtOAc prior to washing 3× with H2O. The combined aqueous layers were extracted once with EtOAc. The organic fractions were combined, washed once with brine, and dried over Na2SO4 prior to concentrating using a rotary evaporator. The residue was chromatographed on silica gel using 75% EtOAc/hexane as the eluent. The resulting promising impure fractions were further purified by silica gel chromatography. A total of 631 mg of the desired N-ethyl-N-4-methoxybenzyl 2,6-dihydroxybenzamide was obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06936590B2
出典データセットuspto-grants-2005_08
ORD IDord-5e527322bbd34ff1bd7734ab74b1d29f
出典メモuspto-grants-2005_08