0100,0100,0100Dear colleagues :
I kindly suggest to establish The Orglist Synthetic Letters, where
simple and facile preparations of the important organic or inorganic
compounds would be presented. The following synthesis is the first
contribution into the forum. This is the original translation from the
czech hanbook published in 1972. The full citation is mentioned
below. Your comments are cordially welcomed.
Preparation of formamidinesulfinic acid
116 g of 30 % hydrogen peroxide weight out in a beaker on
accurate technical balance. Pour the hydrogen peroxide into a
1000 ml beaker and dilute it with 600 ml of distilled water. Place
the beaker into a large vessel (e.g. enameled pot) and encase it
with a mixture of gently grinded ice and sodium chloride. Place the
glass stirrer powered with electric motor into the liquid and under
continuing mixing allow the solution to cool down to 5 °C. Then,
during two hours, under the continuing intensive mixing, add with
spoon small doses of 38 g gently pulverized thiourea. The
temperature during this process should be between 5 and 20 °C.
Refresh the coolant if necessary. When all amount of thiourea is
added continue with cooling of the mixture with ice and sodium
chloride for next 1 hour. Then cool down all mixture close to
freezing point. Filter the separated formamidinesulfinic acid
preferably with small glass frit. Wash obtained product with small
quantity of icy water and then with small portion of methanol.
Washed acid is dried up in vacuum desiccator upon anhydrous
calcium chloride.
Characteristics:
Formamidinesulfinic acid forms the colorless fine needles with
melting point 144 °C. Formamidinesulfinic acid is slightly soluble in
water. Saturated solution contains about 3 % of the acid and pH is
about 5. It is soluble in acetic acid without decomposition. For its
reducing properties the acid is useful in industry. Its ammoniacal
solution rapidly absorbs the oxygen.
Reference:
Klikorka J., Klazar J., Votinsky J., Horak J.: Introduction into
Preparative Inorganic Chemistry, SNTL Publishers, Prague 1972,
page 188 (in Czech).0100,0100,0100
Next: Chemical properties of thiourea-dioxide.
With love,
J.Janovsky
Institute of Chemical Technology
Department of Physical Chemistry
5 Technical Street
Prague, CZ 16628
Czech Republic
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