mmm... NVX swietna lektura!
dla zainteresowanych:
http://rapidshare.de/files/1486421/www. ... utical.rar
(haslo do archiwum:
www.AvaxHome.ru)
A oto przepis na TRETINOIN z powyzszej ksiazki:
Chemical Name: 3,7-dirnethyl-9-(2,6,6-trimethyl-l-cyclohexen-l -yl)-2,4,6,8-nonatetraenoic
acid
Raw Materiais:
Beta-ionol
Triphenylphosph ine hydrobromide
4-Methyl-1 -al-hexadiene-(2,4)-acid-(6)
Manufacturing Process:
100 parts of beta-ionol are dissolved in 200 parts of dimethylforrnamide and after the
addition of 165 parts of triphenylphosphine hydrobromide, stirred for 7 hours at room
temperature. Then 70 parts of 4-rnethyI-l-al-hexadiene-(2,4)-acid-(6) (melting point 177"C,
white needles from water) are added to the now clear solution. 150 parts of isopropanol are added and the whole cooled to -3O'C. Into this solution, while stirring vigorously,
190 parts by volume of a 30?6 solution of sodium methylate in methanol are allowed to
flow in. A vigorous exothermic reaction takes place and the temperature in the interior
of the flask rises to +5"C. It is stirred for another 5 minutes and neutralized with 10% of
sulfuric acid (until acid to Congo).
After stirring for 2 hours at room temperature, the mass of vitamin A acid has crystallized
out. It is sharply filtered off by suction and washed with a little ice-cold isopropanol.
From the filtrate, a further small amount of mainly all trans vitamin A acid crystallizes
out upon the addition of water. The filter cake is suspended in 600 parts of water and
stirred for 4 hours at room temperature; it is filtered by suction and the product washed
with water. It is dried in vacuo at 40' to 50°C and 115 parts of vitamin A acid are obtained.
The melting point lies between 146" and 159°C.
The mixture of the all trans and mainly 9,lO-cis vitamin A acid may be separated by fractional
crystallization from ethanol. All trans vitamin A acid has a melting point of 180"
to 182°C and 9,lO-cis vitamin A acid, which crystallized in the form of pale yellow fine
needles collected into clusters, has a melting point of 189" to 190°C.