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HRID 231252作成日:2026年10月25日

Triphenylphosphine → HCID 20034926、化合物

https://huagongshe.com/reaction/231252

反応式

関与物質

役割名称HCID仕込み量
反応物TriphenylphosphineHCID 11776—
反応物4-Hydroxybenzyl cyanideHCID 26548—
反応物Diethyl azodicarboxylateHCID 5462977—
反応物2-Hydroxymethyl-2-methylcyclohexanoneHCID 11355532—
溶媒BenzeneHCID 241—
溶媒Sodium HydroxideHCID 14798—
生成物HCID 20034926HCID 2003492665%

反応手順

2-Hydroxymethyl-2-methylcyclohexanone [Pearson et al., J. Chem. Soc. Perkin I, 2774, 2778 (1980)] (3.7 g), 4-hydroxybenzyl cyanide (4.49 g) and triphenylphosphine (8.86 g) were dissolved in benzene (100 mL) and cooled in ice under a nitrogen atmosphere. Diethylazodicarboxylate (5.3 mL) was added dropwise and the mixture was allowed to warm to room temperature. The reaction was then refluxed overnight. After cooling to room temperature, the reaction mixture was diluted with 25% aqueous NaOH and extracted with benzene. The extracts were washed with saturated brine solution, dried over MgSO4, filtered and concentrated. The crude residue was chromatographed on SiO2, elution with dichloromethane to give 4.35 g (65% yield) of 2-methyl-2-[[4-(cyanomethyl)phenoxy]methyl]cyclohexanone as an amber oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04845231
出典データセットuspto-grants-1989_07
ORD IDord-b270ecb836b944b4b0260c814845aa6b
出典メモuspto-grants-1989_07