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ChemicalBook CAS DataBase List Potassium di-tert-butyl phosphate

Potassium di-tert-butyl phosphate synthesis

2synthesis methods
Potassium di-tert-butyl phosphate synthesis: Di-tert-butyl phosphite (40.36 mmol) was combined with potassium bicarbonate (24.22 mmol) in 35 ml of water. The solution was stirred in an ice bath and potassium permanganate (28.25 mmole) was added in three equal portions over a period of one hour. The reaction was then allowed to continue for another half hour at room temperature. Decolorizing carbon (600 mg) was then incorporated as the reaction was heated to 60 °C for 15 min. The reaction was then vacuum filtered to remove solid magnesium dioxide. The solid was washed several times with water. The filtrate was then combined with one gram of decolorizing carbon and heated at 60°C for another twenty minutes. The solution was filtered again to give a colorless solution, which was then evaporated in vacuo to give the crude potassium di-tert-butyl phosphate salt.
13086-84-5 Synthesis
DI-TERT-BUTYL PHOSPHITE

13086-84-5
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Yield:-

Reaction Conditions:

with potassium permanganate;Potassium bicarbonate in water monomer at 5 - 20; for 19 h;

Steps:

59

Intermediate 59: Bis(1,1 -dimethylethyl) hydrogen phosphate potassium salt; A solution of bis(1 ,1-dimethylethyl) hydrogen phosphite (100 g, 515 mmol, Alfa Aesar) and potassium bicarbonate (30.9 g, 309 mmol) in water (800 ml) was cooled to 5 0C in an ice bath. To this mixture, potassium permanganate (57.0 g, 360 mmol) was added portionwise over 1 h maintaining the temperature below 20 0C. The reaction mixture was stirred at ambient temperature for 18 h. The reaction was heated to 60 0C and then filtered slowly through a pad of celite. The filtrate was evaporated in vacuo to give the title compound as a white solid (109.7 g); 1H NMR (d6-DMSO) δ 1.26 (18 H, s).

References:

WO2010/122089,2010,A1 Location in patent:Page/Page column 77-78

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