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ChemicalBook CAS DataBase List BENZYLDI-1-ADAMANTYLPHOSPHINE

BENZYLDI-1-ADAMANTYLPHOSPHINE synthesis

2synthesis methods
-

Yield:395116-70-8 4.6 g (12 mmol, 90%)

Reaction Conditions:

with n-butyllithium in toluene;

Steps:

6 Di (1-adamantyl)benzylphosphine:

Example 6 Di (1-adamantyl)benzylphosphine: 4.0 g (13 mmol) of di(1-adamantyl)phosphine were placed in 50 ml of di-n-butyl ether, and 18 ml of a 2.5 M solution of n-BuLi (45 mmol) in toluene were added. The mixture was refluxed for 30 min and cooled and 3.2 g (19 mmol) of benzyl bromide were added dropwise. The mixture was refluxed for 30 min, cooled and washed with saturated ammonium chloride solution (3*), the organic phase was separated off and dried over sodium sulfate and the solvent was distilled off under reduced pressure. Yield: 4.6 g (12 mmol, 90%) of di(1-adamantyl)benzylphosphine. The product is recrystallized from di-n-butyl ether (m.p.: 182° C.) 31P{1H} NMR(162.0 MHz, C6D6, 297 K): δ=29.8 MS: 392.26420 (calc. for C27H37P: 392.26328)

References:

US2004/68131,2004,A1

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