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HRID 382096作成日:2026年10月26日

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

https://huagongshe.com/reaction/382096

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US06307087B1
出典データセットuspto-grants-2001_10
ORD IDord-6ba6ad5d5a97434cac575961b4635e7f
出典メモuspto-grants-2001_10