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HRID 6928作成日:2026年10月23日

Chloroform → 3-[3-(3-Methoxypropyl)-5-(6-phenylpyridin-3-yl)-1,2,4-triazol-4-yl]-2-methylbenzamide

https://huagongshe.com/ja/reaction/6928

反応式

関与物質

役割名称HCID仕込み量
反応物ChloroformHCID 6212—
反応物Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 18462—
反応物3-Amino-2-methylbenzamideHCID 16495773—
反応物5-[5-(3-Methoxypropyl)-1,3,4-oxadiazol-2-yl]-2-phenylpyridineHCID 22019236—
溶媒1,3-Dimethyl-2-imidazolidinoneHCID 6661—
生成物3-[3-(3-Methoxypropyl)-5-(6-phenylpyridin-3-yl)-1,2,4-triazol-4-yl]-2-methylbenzamideHCID 2201925156.1%

反応条件

温度200 °C

反応手順

5-[5-(3-Methoxypropyl)-1,3,4-oxadiazol-2-yl]-2-phenylpyridine (1.0 g) prepared in the Reference Example 7 was dissolved in 1,3-dimethyl-2-imidazolidinone (10 ml), followed by addition of 3-amino-2-methylbenzamide (1.53 g) prepared in the Reference Example 6 and D-10-camphorsulfonic acid (290 mg), and stirred at 200° C. for 16 hours. After the reaction solution was cooled to ambient temperature, chloroform was added to the solution, which was then washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: chloroform/methanol=10/1), to afford the entitled compound (812 mg, 56%). The physico-chemical values are as follows.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07084164B2
出典データセットuspto-grants-2006_08
ORD IDord-1220b742e04a4582a13bd0b0471941a4
出典メモuspto-grants-2006_08