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HRID 963575作成日:2026年10月26日

Water → 4,4-Bis(Hydroxymethyl)Biphenyl

https://huagongshe.com/reaction/963575

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sulfuric AcidHCID 1118—
反応物TetrahydrofuranHCID 8028—
反応物Dimethyl 4,4'-biphenyldicarboxylateHCID 13099—
反応物Aluminium lithium hydrideHCID 21226445—
生成物4,4-Bis(Hydroxymethyl)BiphenylHCID 6874350193%

反応条件

温度-20 °C

反応手順

In a 1000 ml three-necked flask, fitted with an efficient condenser, a thermometer and a dropping funnel, is placed a suspension of 6,2 g (0.144 mol) LiAlH4 in 80 ml dry THF under an inert atmosphere. A solution of 30 g (0.122 mol) dimethyl 4,4'-biphenyldicarboxylate in 250 ml dry THF is added dropwise over a period of 30 minutes. The mixture is refluxed with stirring for 1 hour. The mixture is cooled to -20° C. and 80 ml of H2O is added dropwise, followed by slow addition of 80 ml of 20% H2SO4 (aq.). The THF is evaporated under reduced pressure to give a suspension of colourless product in aqueous acid. The product is filtered and washed with H2O. After recrystallisation from aceton, white crystals are obtained. Yield: 93%; melting point: 187.3° C.-188.5° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05763539
出典データセットuspto-grants-1998_06
ORD IDord-63b2289b48a74ce58fc15c0884e38cf7
出典メモuspto-grants-1998_06