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ChemicalBook CAS DataBase List (OXYDI-2,1-PHENYLENE)BIS(DIPHENYLPHOSPHINE)
166330-10-5

(OXYDI-2,1-PHENYLENE)BIS(DIPHENYLPHOSPHINE) synthesis

2synthesis methods
-

Yield:166330-10-5 87%

Reaction Conditions:

Stage #1: diphenyletherwith n-butyllithium in hexane at -78 - 25; for 17 h;
Stage #2: chloro-diphenylphosphine in hexane at 20; for 16 h;Cooling with ice;

Steps:

1.1; 1.2

Diphenyl ether (0.02 mol) was diluted in hexane (50 mL), and a solution of n-BuLi (42 mmol) in hexane was added dropwise (about 5 min) at -78 ° C. The reaction was carried out for 1 h, and then To room temperature (about 25 ° C), and continue to stir for 16h;(2) Then 15 mL of a solution of diphenylphosphine chloride (42 mmol) in n-hexane was added dropwise to the reaction system of step (1) in an ice-water bath, and the reaction was continued at room temperature (about 25 ° C). The reaction was stirred for 16 h under reduced pressure; the solvent was removed by rotary evaporation to obtain a pale yellow viscous oil, which was washed with acetone and dried under vacuum to obtain 9.4 g of a white powder, which is the compound represented by formula (3-1): the yield was 87%

References:

CN110386956,2019,A Location in patent:Paragraph 0294; 0296; 0298; 0299

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