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HRID 47610作成日:2026年10月25日

Methyl acetoacetate → HCID 178490910、化合物

https://huagongshe.com/reaction/47610

反応式

関与物質

役割名称HCID仕込み量
反応物Methyl acetoacetateHCID 7757—
反応物TriethylamineHCID 8471—
反応物(4-Methoxybenzyl)hydrazine dihydrochlorideHCID 22747476—
溶媒TolueneHCID 1140—
生成物HCID 178490910HCID 178490910—

反応条件

温度100 °C

反応手順

A solution containing 2.75 g of (4-methoxybenzyl)hydrazine dihydrochloride in 50 ml of toluene was treated with 1.7 ml of triethylamine at rt and then stirred for 5 min. The mixture was then treated with 1.32 ml of methyl acetoacetate and heated at 100° C. for 15 min. The solvent was evaporated under reduced pressure and then the residue partitioned between dichloromethane/10% citric acid and extracted three times. Combined extracts were washed with brine, then dried over anhydrous magnesium sulphate, filtered and evaporated to give a yellow solid. The solid was purified by flash chromatography on silica gel using methanol/dichloromethane (1:49) for the elution to give 2.3 g of 2-(4-methoxybenzyl)-5-methyl-2H-pyrazol-3-ol as a white solid. Mass spectrum (ES) m/z 219 [M+H]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06699887B2
出典データセットuspto-grants-2004_03
ORD IDord-5779c6194f914b70860d7ff1cb025ff6
出典メモuspto-grants-2004_03