33494-81-4

White powder

Di-tert-butyl phosphate (dtbp-H) is used with metal acetates in a high-yield synthetic procedure for the preparation of transition metal phosphate cages [M4(μ4-O)(dtbp)6] (M = Co, Zn).

Flammable

General procedure for the synthesis of di-tert-butyl phosphate from di-tert-butyl phosphite: To an aqueous solution (170 ml) containing di-tert-butyl phosphite (38.8 g, 0.2 mol) and potassium bicarbonate (12.2 g, 0.12 mol), add finely pulverized potassium permanganate (23.1 g, 0.14 mol) in batches with stirring and under effective cooling (ice-salt bath) for about 1 hour. . The reaction temperature was maintained at 0°C to control the exothermic reaction. After addition, stirring was continued at room temperature for 30 minutes. Subsequently, the mixture was heated to 60°C and maintained for 15 minutes to promote coagulation of the manganese dioxide colloidal suspension, after which the manganese dioxide was removed by filtration. The filtrate was decolorized by boiling with the addition of activated carbon (3 g). The decolorized filtrate was used directly in the next step of the reaction. Concentrated hydrochloric acid (35 mL) was slowly added to the above filtrate under stirring and external cooling (0-5 °C) to induce precipitation of compound 2. The colorless crystalline precipitate was collected by filtration, washed with a small amount of ice water and finally dried under vacuum in the presence of phosphorus pentoxide to give compound 3 (40.0 g, 95% yield).

[1] Patent: WO2013/19169, 2013, A1. Location in patent: Paragraph 0227; 0228
[2] Patent: WO2008/14602, 2008, A1. Location in patent: Page/Page column 59
[3] Patent: WO2012/35548, 2012, A1. Location in patent: Page/Page column 39
[4] Patent: US2013/178443, 2013, A1. Location in patent: Paragraph 0932; 0933
[5] Patent: US2013/172249, 2013, A1. Location in patent: Paragraph 0295