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HRID 1269928作成日:2026年10月27日

Cyanomethylenetributylphosphorane → HCID 178503317、化合物

https://huagongshe.com/reaction/1269928

反応式

関与物質

役割名称HCID仕込み量
反応物CyanomethylenetributylphosphoraneHCID 4622928—
反応物4-(methylthio)-1H-indazol-5-olHCID 22933648—
反応物tert-butyl 4-{[4-(methylsulfonyl)-1H-indazol-5-yl]oxy}azepane-1-carboxylateHCID 22933794—
反応物HCID 178515017HCID 178515017—
溶媒TolueneHCID 1140—
生成物HCID 178503317HCID 17850331758%

反応条件

温度100 °C

反応手順

The 4-(methylthio)-1H-indazol-5-ol (0.166 g, 0.92 mmol) obtained in Example 607 and the trans-2-(4-hydroxycyclohexyl)-1H-isoindole-1,3(2H)-dione (0.151 g, 0.61 mmol) obtained in Example 323, (a) were added to a solution of cyanomethylenetri-n-butylphosphorane (0.247 g, 0.92 mmol) in toluene (6 ml), and the resulting mixture was heated at 100° C. and stirred for 7 hours. The reaction solution was concentrated and then diluted with chloroform, and a 1N-aqueous sodium hydroxide solution was added thereto, followed by extraction with chloroform (three times). The extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1˜1/1) to obtain 2-(cis-4-{[4-(methylthio)-1H-indazol-5-yl]oxy}cyclohexyl)-1H-isoindole-1,3(2H)-dione (0.144 g: 58%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07199147B2
出典データセットuspto-grants-2007_04
ORD IDord-45618f7a7ec74444834daa30315ddd74
出典メモuspto-grants-2007_04