ChemicalBook CAS DataBase List Bis(di-tert-butyl)-4-dimethylaminophenylphosphine

Bis(di-tert-butyl)-4-dimethylaminophenylphosphine synthesis

6synthesis methods

Product Name:Bis(di-tert-butyl)-4-dimethylaminophenylphosphine
CAS Number:932710-63-9
Molecular formula:C16H28NP
Molecular Weight:265.37

13716-10-4 Synthesis

13716-10-4
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Magnesium, chloro[4-(dimethylamino)phenyl]-

108949-55-9
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Bis(di-tert-butyl)-4-dimethylaminophenylphosphine

932710-63-9
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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

13716-10-4 Synthesis

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