DI-TERT-BUTYLPHENYLPHOSPHINE synthesis

Yield:32673-25-9 94.7%

Reaction Conditions:

Stage #1:bromobenzene with magnesium in tetrahydrofuran for 2 h;Inert atmosphere;Reflux;
Stage #2:di(tert-butyl)chlorophosphine with tetrakis(triphenylphosphine) palladium⁽⁰⁾ in tetrahydrofuran at 20; for 3 h;Reflux;Inert atmosphere;

Steps:

1 Example 1. Preparation of di-tert-butylphenylphosphine
Under nitrogen protection,1L three bottles,From 27 g of bromobenzene,5 g of magnesium turnings and 400 mlIn dry THFTo produce a Grignard reagent,Refluxed for 2 hours,Down to room temperature,2 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 10 minutes,33 g of di-tert-butylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 3 hours.And the mixture was added dropwise to the reaction solution under ice-water bath200 mL of saturated aqueous ammonium chloride was quenched,Liquid separation,Organic phase, dissolved, add methanol crystallization,And filtered to obtain 36 g of di-t-butylphenylphosphine as white,Yield 94.7%.

References:

Panjin Gelin Kaimo Technology Co., Ltd.;Rao, Zhihua;Gong, Ningrui CN105859774, 2016, A Location in patent:Paragraph 0058; 0059; 0060; 0061

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