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ChemicalBook CAS DataBase List 2-DI-TERT-BUTYLPHOSPHINO-2',4',6'-TRIISOPROPYLBIPHENYL

2-DI-TERT-BUTYLPHOSPHINO-2',4',6'-TRIISOPROPYLBIPHENYL synthesis

2synthesis methods
13716-10-4 Synthesis
Di-tert-butylchlorophosphane

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

21524-34-5 Synthesis
1-BROMO-2,4,6-TRIISOPROPYLBENZENE

21524-34-5
269 suppliers
$6.00/5g

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Yield:564483-19-8 94%

Reaction Conditions:

Stage #1: 2-bromo-1-chlorobenzene;2,4,6-triisopropyl-1-bromobenzenewith magnesium in tetrahydrofuran; for 2 h;Inert atmosphere;Reflux;
Stage #2: di(tert-butyl)chlorophosphinewith tetrakis(triphenylphosphine) palladium(0) in tetrahydrofuran at 20; for 5.5 h;Reflux;Inert atmosphere;Reagent/catalyst;

Steps:

5 Example 5 Preparation of 2'-di -tert-butylphosphino-2,4,6-triisopropylbiphenyl

1L three bottles,To a solution of 32.5 g of 2,4,6-triisopropylbromobenzene,5.6 g of magnesium turnings and 300 mL of anhydrous THF,20 g of o-chlorobromobenzene was dropwise added,2,4,6-triisopropyl-2-bromobiphenyl Grignard reagent,Refluxed for 2 hours,Down to room temperature,2.4 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 30 minutes,18.8 g of di-tert-butylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 5 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,And filtered to obtain 41.7 g of white 2-di-tert-butylphosphine-2,4,6-triisopropylbiphenyl,Yield 94%.

References:

CN105859774,2016,A Location in patent:Paragraph 0078; 0079; 0080; 0081

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