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Tbaf, 3h2o

  1. Jun 16, 2011 #1
    Dear Sir,

    We have been manufacturing tetrabutylammonium fluoride (TBAF) 1M solution in THF (tetrahydrofuran). Our quality is very good and has been accepted by few MN pharma companies.

    We have also been able to produce TBAF, 3H20 (TBAF trihydrate) with +99% purity and other specs such as water content is also well within the range. The only problem we are facing is we have not been able to get the solid material or at least semi-solid or chunk type. The compound is reported as solid having purity 97-99% and mp 58-63 deg C. Our product remains as thick viscous light yellowish brown liquid. Even after cooling to 0 deg C, it does not solidify.

    We did literature survey and one of the papers says-Sometimes the product did not solidify after completing the reaction. In that case one can prepare its solution in water with conc. of 13 to 14% (~0.5 M), cool to 5 deg C, The white solids obtained are reported as a clathrate of TBAF, 38.5 H2O. The solids are then filtered, washed with cold water and air-dried. This compound has mp of 30 deg C. The water of crystallization can be removed under vaccum at < 50 deg C.

    We feel this is good for lab scale preparation but may not be good for commercial production such as 500 to 1000 Kg.

    How could we get solid TBAF, 3H2O? Could somebody guide us?

    Milind Garkhedkar.
     
  2. jcsd
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