![](/CAS/GIF/932710-63-9.gif)
Bis(di-tert-butyl)-4-dimethylaminophenylphosphine synthesis
- Product Name:Bis(di-tert-butyl)-4-dimethylaminophenylphosphine
- CAS Number:932710-63-9
- Molecular formula:C16H28NP
- Molecular Weight:265.37
![Di-tert-butylchlorophosphane](/CAS/GIF/13716-10-4.gif)
13716-10-4
257 suppliers
$22.00/1g
![Magnesium, chloro[4-(dimethylamino)phenyl]-](/CAS/20211123/GIF/108949-55-9.gif)
108949-55-9
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![Bis(di-tert-butyl)-4-dimethylaminophenylphosphine](/CAS/GIF/932710-63-9.gif)
932710-63-9
223 suppliers
$11.00/250mg
Yield:932710-63-9 85%
Reaction Conditions:
Stage #1: di(tert-butyl)chlorophosphine;4-N,N-dimethylaminophenyl magnesium chloride at -30; for 0.166667 h;Inert atmosphere;
Stage #2: with ammonium chloride in water at -30; for 0.5 h;
Steps:
1
The reaction system is cooled to -30 ° C, under the protection of nitrogen flow,Adding catalyst to remove water by vacuum dryingAfter the powder was 10.2 g, the reaction was stirred for 10 min.Further, 930 g of di-tert-butylphosphonium chloride was added dropwise.The dropping process controls the reaction temperature below -30 ° C, and the dropwise addition is completed, and the temperature is raised to 50 ° C for 3 hours to obtain di-tert-butyl-4-dimethylaminophenylphosphine. The reaction system was again cooled to -30 ° C, and 1.5 L of a saturated aqueous solution of ammonium chloride was added dropwise with stirring.After stirring for 0.5 h, the mixture was allowed to stand for stratification under the protection of a nitrogen stream.The liquid is separated, and the upper organic phase is concentrated and concentrated to obtain a yellow viscous material for high vacuum distillation under reduced pressure.The degree of vacuum is 0.3-0.5 mmHg, and the fraction of 120 ° C - 140 ° C is collected, and after cooling, it is an off-white solid.That is, the ligand di-tert-butyl-4-dimethylaminophenylphosphine has a yield of 1145-1160 g, a purity of not less than 97%, and a yield of 81.5% to 85.0%.
References:
CN108659054,2018,A Location in patent:Paragraph 0057; 0059; 0060
![Di-tert-butylchlorophosphane](/CAS/GIF/13716-10-4.gif)
13716-10-4
257 suppliers
$22.00/1g
![4-(N,N-DIMETHYL)ANILINEMAGNESIUM BROMIDE](/CAS/GIF/7353-91-5.gif)
7353-91-5
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$226.00/50mL
![Bis(di-tert-butyl)-4-dimethylaminophenylphosphine](/CAS/GIF/932710-63-9.gif)
932710-63-9
223 suppliers
$11.00/250mg
![Di-tert-butylphosphine](/CAS/GIF/819-19-2.gif)
819-19-2
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$74.00/1g
![4-Bromo-N,N-dimethylaniline](/CAS/GIF/586-77-6.gif)
586-77-6
422 suppliers
$5.00/10g
![Bis(di-tert-butyl)-4-dimethylaminophenylphosphine](/CAS/GIF/932710-63-9.gif)
932710-63-9
223 suppliers
$11.00/250mg
![4-CHLORO-N,N-DIMETHYLANILINE](/CAS/GIF/698-69-1.gif)
698-69-1
66 suppliers
$17.00/250mg
![Bis(di-tert-butyl)-4-dimethylaminophenylphosphine](/CAS/GIF/932710-63-9.gif)
932710-63-9
223 suppliers
$11.00/250mg
![4-Bromo-N,N-dimethylaniline](/CAS/GIF/586-77-6.gif)
586-77-6
422 suppliers
$5.00/10g
![Bis(di-tert-butyl)-4-dimethylaminophenylphosphine](/CAS/GIF/932710-63-9.gif)
932710-63-9
223 suppliers
$11.00/250mg