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HRID 1296994作成日:2026年10月27日

Chlorodicyclohexylphosphine → 2-(Dicyclohexylphosphino)-2'-methoxybiphenyl

https://huagongshe.com/reaction/1296994

反応式

関与物質

役割名称HCID仕込み量
反応物ChlorodicyclohexylphosphineHCID 2734135—
反応物3-Methyl-1,1-bis(4-methylphenyl)-2-butanoneHCID 12040744—
反応物ButyllithiumHCID 178418339—
溶媒TetrahydrofuranHCID 8028—
生成物2-(Dicyclohexylphosphino)-2'-methoxybiphenylHCID 1179418654.4%

反応手順

A solution of 1 (535 mg, 2.03 mmol) in THF (20 mL) was cooled to −78° C. under argon, then n-BuLi (1.6 M in hexane, 1.35 mL, 2.16 mmol) was added dropwise. After 2.5 h at −78° C., a solution of chlorodicyclohexylphosphine (570 mg, 2.45 mmol) in THF (3 mL) was added over 10 min. The reaction mixture was then allowed to warm to room temperature overnight, then quenched with saturated aqueous NaHCO3 and concentrated in vacuo. The resulting aqueous suspension was extracted with ether (2×50 mL), and the combined ethereal layers were dried (Na2SO4), filtered and concentrated in vacuo. The resulting crude solid was recrystallized from ethanol to afford 420 mg (54%) of a white solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07247731B2
出典データセットuspto-grants-2007_07
ORD IDord-fe8460489d354aa6ae274ba3b356465a
出典メモuspto-grants-2007_07