ChemicalBook CAS DataBase List X-PHOS

X-PHOS synthesis

3synthesis methods

Product Name:X-PHOS
CAS Number:564483-18-7
Molecular formula:C33H49P
Molecular Weight:476.72

21524-34-5 Synthesis

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

16523-54-9 Synthesis

16523-54-9
271 suppliers
$8.00/1g

583-53-9
316 suppliers
$10.00/5g

564483-18-7
396 suppliers
$5.00/250mg

Yield:564483-18-7 89%

Reaction Conditions:

Stage #1: 2,4,6-triisopropyl-1-bromobenzenewith n-butyllithium in tetrahydrofuran at 0; for 1 h;Inert atmosphere;
Stage #2: 2,3-dibromobenzene in tetrahydrofuran at 0; for 1 h;Inert atmosphere;
Stage #3: chlorodicyclohexylphosphaneFurther stages;

Steps:

4 Example 4

Under the protection of nitrogen, 200 ml of THF and 31g of 2, 4, 6-tri-isopropyl-bromobenzene was added to 1L three-mouth bottle. The temperature was cooled down to 0 °C, and 46 ml of 2.5M n-butyl lithiumwas added dropwise. The reaction was continued for 1 hour after the addition. At 0 °C, 24.6g O-dibromobenzene was added dropwise. The reaction was continued for 1 hour after the addition. At0 °C, 42 ml of 2.5M n-butyl lithiumwas added dropwise to the reaction liquid.After the addition, the reaction was continued for 1 hour. 26.7g of dicyclohexyl phosphine was added dropwise, and the temperature was naturally warmed to react at room temperature for 2 hours. 200 ml saturated ammonium chloride aqueous solution was added dropwsie to the reaction liquid under the ice bath to quench the reaction. After phase separation, the organic phase was precipitated, and methanol was added for crystallization. Byfiltering, 44.5g white product of 2’-dicyclohexyl phosphino-2, 4, 6-tri-isopropyl biphenyl was obtained, with a yield of 89%.

References:

CN105273006,2016,A Location in patent:Paragraph 0069; 0070

694-80-4 Synthesis