ChEBI: Deuterium atom is the stable isotope of hydrogen with relative atomic mass 2.014102 and a natural abundance of 0.0115 atom percent (from Greek deltaepsilonupsilontauepsilonrhoomicronnu, second). It contains a deuteron.
About 150 ml. of n-butyl ether, dried over Na, is distilled into
the reaction flask and 5.75 g. of LiAlH4 (40% excess) is then added
under a nitrogen blanket. The mixture is frozen with liquid N s.
The apparatus is then evacuated, and the flask contents are
brought to boiling by careful heating. After 1.5 hours, it is again cooled with liquid Ns
, the evacuation is repeated, and 5 ml. of
99.5% D2O is added to the solidified mixture, using
a hypodermic syringe to pierce the rubber cap. Because of the low reaction temperature, the flask
becomes coated with ice on the outside. By repeated immersion
in liquid N3, the temperature is controlled so that the ice on the
outer wall of the flask does not melt. As soon as the reaction
subsides somewhat, two additional portions of 6.5 ml. of DSO
each are added (for a total of 18 ml. or 150% excess). The yield
is 10 liters of HD. The purity is 97-99%.
LiAlH4 + 4D2O = LiOD + Al(OD)3 + 4HD
