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ChemicalBook CAS DataBase List 2-(Di-tert-butylphosphino)biphenyl

2-(Di-tert-butylphosphino)biphenyl synthesis

6synthesis methods
13716-10-4 Synthesis
Di-tert-butylchlorophosphane

13716-10-4
254 suppliers
$22.00/1g

2052-07-5 Synthesis
2-Bromobiphenyl

2052-07-5
385 suppliers
$16.30/1g

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Yield:224311-51-7 95.7%

Reaction Conditions:

Stage #1: 2-Bromobiphenylwith magnesium in tetrahydrofuran; for 2 h;Inert atmosphere;Reflux;
Stage #2: di(tert-butyl)chlorophosphinewith tetrakis(triphenylphosphine) palladium(0) in tetrahydrofuran at 20; for 2 h;Reflux;Inert atmosphere;Reagent/catalyst;

Steps:

2 Example 2. Preparation of 2- (di-t-butyl phosphino) biphenyl

Under nitrogen protection,1L three bottles,From 40 g of 2-bromobiphenyl,5 g of magnesium turnings and 400 ml of anhydrousTHF to produce Grignard reagent,Refluxed for 2 hours,Down to room temperature,2 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 30 minutes,33 g of di-tert-butylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 2 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,The organic phase is dissolved,Add methanol crystallization,Filtration gave 49 g of white 2- (di-tert-butylphosphine) biphenyl, and the yield was 95.7%.

References:

CN105859774,2016,A Location in patent:Paragraph 0062; 0063; 0064; 0065; 0066; 0067; 0068; 0069

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