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HRID 252237作成日:2026年10月26日

Diisopropylethylamine → HCID 58230870、化合物

https://huagongshe.com/reaction/252237

反応式

関与物質

役割名称HCID仕込み量
反応物DiisopropylethylamineHCID 81531—
反応物4-Amino-3-hydroxybenzoic acidHCID 137566—
反応物2-Methylpyridine-3-carbonyl chlorideHCID 12902598—
溶媒DichloromethaneHCID 6344—
溶媒TetrahydrofuranHCID 8028—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 58230870HCID 5823087040.2%

反応条件

温度0 °C

反応手順

2-methyl nicotinoyl chloride (0.2 g, 0.00128 mols) is dissolved in 30 ml dry DCM and N,N′-Diisopropylethylamine (0.994 g, 0.00769 mols) is added slowly to the acid chloride solution at 0° C. under nitrogen atmosphere. A solution of 4-Amino-3-hydroxybenzoic acid (0.196 g, 0.00128 mols) in 10 ml dry THF is slowly added to the above solution at 0° C. The solution is then stirred at 0° C. for 30 mins and then at RT overnight. The reaction mixture is then diluted with 100 ml Ethyl acetate and stirred for 30 mins. The precipitated tarry material is filtered off over celite bed and the organic phase given 4×20 ml water wash, 2×10 ml brine wash dried over sodium sulfate and rotary evaporated to get the crude amide (140 mg) which is taken for the cyclisation step without further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07868033B2
出典データセットuspto-grants-2011_01
ORD IDord-68113f6b2507438c962f16b003e8b0f2
出典メモuspto-grants-2011_01