Dibenzyl phosphite synthesis
- Product Name:Dibenzyl phosphite
- CAS Number:17176-77-1
- Molecular formula:C14H15O3P
- Molecular Weight:262.24
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Example 15 Synthesis of dibenzylphosphonate 15: Phenol 14 (0.51 g, 0.95 mmol) was dissolved in CH3CN (8 mL) and Cs2CO3 (0.77 g, 2.37 mmol) and trifluoromethanesulfonate (0.8 g, 1.90 mmol) were added sequentially. The reaction mixture was stirred at room temperature for 1.5 h and then concentrated under reduced pressure to remove the solvent. The residue was subjected to liquid-liquid partitioning with EtOAc and saturated NaCl solution. The organic phase was dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (eluent: 3% MeOH/CH2Cl2) to afford dibenzylphosphonate 15 (0.62 g, 80% yield) as a white solid.
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Yield:17176-77-1 86.6%
Reaction Conditions:
with sodium methylate at 140; under 9.0009 Torr;Reflux;Inert atmosphere;
Steps:
5 Example 5
In a nitrogen-protected 1 L round bottom three-necked flask, 110 g of dimethyl phosphite, 325.2 g of benzyl alcohol, and 2.2 g of MeONa were added; the temperature was raised to reflux with stirring, and a fraction (methanol) of 60 to 65 ° C was collected, and then the bottom temperature of the kettle was set to 140 ° C. At 1.2kPa, the temperature was further increased to reflux, and the second stage fraction (excess benzyl alcohol) was distilled off, and the crude di (benzyl) phosphite was obtained at the bottom of the kettle; the crude dibenzyl phosphite was further washed with water, and 500 ml of It was extracted with methyl chloride, dried over anhydrous sodium sulfate, and after desolvation, 235.6 g of dibenzyl phosphite with a purity of 96.4% was obtained with a yield of 86.6%.
References:
Sichuan Fusida Bio-technology Development Co., Ltd.;Liu Hu;Yang Lu;Li Zhou;Wang Wen;Zhang Xian CN110669069, 2020, A Location in patent:Paragraph 0027
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