Toluene → Methanefluorodiphosphonate

Temperatur

41 °C

To a stirred solution of tetraisopropyl fluoromethylenediphosphonate (320 mg, 0.88 mmol) in 1,2-dichloroethane (5 mL) was added dropwise trimethylsilyl bromide (0.70 mL, 5.28 mmol). The resulting solution was stirred at 40-42° C. for 24 h and 3 mL of anhydrous toluene was added. The mixture was concentrated to dryness, and coevaporated with toluene once. The residue was redissolved in DMF (3 mL)/water (2 mL) mixture and concentrated. The residue was mixed with DMF (2 mL) and tributylamine (0.42 mL, 1.76 mmol) and then concentrated to dryness. The residue was coevaporated with anhydrous DMF two times. The resulting residue was dried in a vacuum oven at 30° C. overnight to give a slightly yellow residue (460 mg).

1. concentrationThe mixture was concentrated to dryness
2. dissolutionThe residue was redissolved in DMF (3 mL)/water (2 mL) mixture
3. concentrationconcentrated
4. concentrationconcentrated to dryness
5. customThe resulting residue was dried in a vacuum oven at 30° C. overnight

ORD-Eintrag

ord-001da96a64ec4180911e9d50ff0a49b6

Quelldatensatz

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07598230B2