Refrigerated dropping funnel and reflux condenser

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and Reflux Condenser The apparatus in the figure (0.25scale) consists of a refrigerated dropping funnel b-d and a reflux condenser b , f, e. This onepiece apparatus has pmved useful in in the eanGolline the temoerature of a reaeent (e.e.. concentrated hvdroeen " - oerodde . and related nrennration of oe&avtrifluoraeetie in :he Baever-Villieer reaction , ~ ~ &id ~ ~ ~ ~ , ~ nndatiun ufaromatic compounds1) dnnng additmn to a refluxma reaction mixture. A cold environment may be maintained hy addmg ice or ice and salt to water contained in chamber a. Lower temperatures are achieved with Dry Ice or Dry Ice a s a slurry with acetone or alcohol. The apparatus was c o n s t ~ c t e dh m a 2-L, heavy-walled beaker a,standard-taper, 24/40,outerjoints b , 25-mm OD tubing c, stopcock with Teflon plugd, and a standardtaper, 24/40,O-ring, inner joint e. Three expansion bulbs (45 mm ad.) were added to the reflux condenser f to ~ r o v i d eadditonal surface area. The solid rods a t n were needed, during eonstrueti&, to hold parts b-d and b , f, e. These latter part; were connected by cross-over tube h while the ring seals a t i were being made. This tube serves as a stabilizine brace and oermits flow of .. eas.. ifan inert atmomhere is used. If excesswe rtrams develop dunng ronstrurtion, the solid rods at g may he cut. Asmall hole 10-12 mm, is hlown near the honom o f a and s h ~ h t l ylarger diameter tuhing is forced into the hole to serve u.i a drain ~

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'chambers, R. D.; Gaggin, P.: Musgrave, W. K. R. J. Chem. Soc. 1959.1804. 2~orrespanding author

M. D. Cagle, T. Denton, and E. J. ~isenbraun~ Oklahoma State University Stillwater, OK 74078

Volume 69

Number 4 April 1992

331

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