Tributylamine → Difluoromethylene diphosphonate

Temperature

41 °C

To a stirred solution of tetraisopropyl difluoromethylenediphosphonate (2.0 g, 5.26 mmol) in anhydrous acetonitrile (30 mL) was added dropwise trimethylsilyl bromide (4.17 mL, 31.58 mmol). The resulting solution was stirred at 40-42° C. for 24 h, concentrated to dryness, and coevaporated with anhydrous acetonitrile once. The residue was re-dissolved in an acetonitrile/water mixture, and then coevaporated with DMF. The residue was dissolved in a DMF solution of tributylamine (1.93 g, 2.48 mL, 10.43 mmol), transferred into multiple small flasks, concentrated to dryness, and coevaporated with anhydrous DMF three times. The residue was dried in a vacuum oven at 40° C. for 4 h to give a slightly yellow residue (3.35 g).

1. concentrationconcentrated to dryness
2. dissolutionThe residue was re-dissolved in an acetonitrile/water mixture
3. customtransferred into multiple small flasks
4. concentrationconcentrated to dryness
5. customThe residue was dried in a vacuum oven at 40° C. for 4 h

ORD record

ord-7fa1df5cd85944779df427feb22463b3

Source dataset

uspto-grants-2007_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07285658B2