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HRID 1443472作成日:2026年10月26日

Sodium Hydroxide → 4-Methoxy-3-methyl-2-[(5-methyl-pyridine-2-carbonyl)-amino]-benzoic acid methyl ester

https://huagongshe.com/reaction/1443472

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium HydroxideHCID 14798—
反応物Phosphorus oxychlorideHCID 24813—
反応物5-Methylpicolinic acidHCID 199575—
反応物Methyl 2-amino-4-methoxy-3-methylbenzoateHCID 59165444—
溶媒PyridineHCID 1049—
溶媒DichloromethaneHCID 6344—
生成物4-Methoxy-3-methyl-2-[(5-methyl-pyridine-2-carbonyl)-amino]-benzoic acid methyl esterHCID 5768722465.2%

反応手順

2-Amino-4-methoxy-3-methyl-benzoic acid methyl ester (400 mg, 2 mmol) and 5-methyl-pyridine-2-carboxylic acid (280 mmol, 2 mmol) where dissolved in dichloro-methane (8 ml) and pyridine (1 ml). Phosphorous oxychloride (0.37 ml) was added while cooling on ice-bath. The mixture was left at 0° C. for 1 h then allowed to attain room temperature. Aqueous sodium hydroxide (20 ml, 1M) was added and the mixture were extracted with dichloromethane. Purification by column chromatography on silica gel (ether-pentane 1:1) gave pure title compound (410 mg, 65%). MS (M−H)+ 315.1

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07659245B2
出典データセットuspto-grants-2010_02
ORD IDord-b88460349c4342418e3e686e5aa8d14c
出典メモuspto-grants-2010_02