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HRID 426533作成日:2026年10月26日

Potassium Hydroxide → HCID 20391041、化合物

https://huagongshe.com/reaction/426533

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium HydroxideHCID 14797—
反応物N-(3-chloropropyl)piperidine hydrochlorideHCID 79624—
反応物2,7-Dihydroxyfluoren-9-oneHCID 4354181—
溶媒WaterHCID 962—
溶媒TolueneHCID 1140—
生成物HCID 20391041HCID 20391041—

反応手順

A mixture of 63.6 g (0.30 mole) of 2,7-dihydroxy-fluoren-9-one, 188 g (0.95 mole) of 1-(3-chloropropyl) piperidine hydrochloride, 132 g (2.0 mole) of 85% potassium hydroxide in 900 ml of toluene and 300 ml of water is refluxed with vigorous stirring for 20 hours. The layers are separated upon cooling and the organic layer is washed 3 times with water, once with a saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. The mixture is filtered and the solvent removed in vacuo. The residue is taken up in isopropyl alcohol and acidified to Congo Red with ethereal hydrogen chloride. The solid which precipitates is filtered, recrystallized from a mixture of 3 parts isopropyl alcohol to 1 part methanol, and the 2,7-bis(3-piperidinopropoxy)fluoren-9-one dihydrochloride so prepared is dried at 100° C. for 24 hours under vacuum, m.p. 279.5°-80.5° C., λmaxH2O 270, and E1cm1% 1370.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04169897
出典データセットuspto-grants-1979_10
ORD IDord-360135aef7d54317bbf552753ebe0a2f
出典メモuspto-grants-1979_10