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33748292604
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note
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31P NMR. After completion of the reaction (approximately 2 h) the solution was evaporated to dryness. The crude product was subjected to several crystallizations from dichloromethane to give pure 1a and 1b with a yield above 90%. Synthesis of phosphate 2: 1.9 g (5 mmol) of 1-hydroxyphosphonate 1a and 0.5 g (5 mmol) of triethylamine in dry acetonitrile (40 mL) were heated in a sealed glass ampoule for 15 h at 65 °C. The crude product precipitated at room temperature, then was filtered off and crystallized from dichloromethane/toluene or toluene to give 2 in 96% yield.
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31
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33748334842
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note
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6)...
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32
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33748317605
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note
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o > 4σ, collected on Smart APEX (Bruker) at 300 K. Crystallographic data have been deposited at the Cambridge Crystallographic Data Centre, Cambridge, UK. Copies of the data can be obtained, free of charge, on application to CCDC, 12 union Road, Cambridge CB2 1EZ, UK [fax: +44 (0) 1223 336033 or e-mail deposit@ccdc.cam.ac.uk].
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33
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