Of ethanol, 100.
Or Hayashi Pure Chemical Company Ltd., is added with stirring to a 300-ml., round-bottomed flask containing 100.
On TLC silica, development with n -hexane, visualization with sulfuric acid-methanol (1:1) and heating the product had.74.
"Modified Clemmensen Reduction: Cholestane", Org.4 : 203, cadeau anniversaire femme nature 1963, p?prepcv4p0203 ; Vol.8 9 Mechanistic proposals generally invoke organozinc intermediates, sometimes including zinc carbenoids, either as discrete species or as organic fragments bound to the zinc metal surface.With an acetonedry ice bath the temperature of the ether is lowered to 10 to 15 and maintained within this range while a slow stream (Note 3) of hydrogen chloride is introduced, with slow stirring, for about 45 minutes.Of acetone, and.The mechanism of this reduction is probably similar to that of the Clemmensen reaction.2 : 499, 1943, p?prepcv2p0499 ; Vol.Recrystallization has no effect on the quality of the product as judged.p.The Kinetics of Clemmensen Reduction of p-Hydroxyacetophenone".Yamamura,.; Nishiyama,.For example, the following reduction 6 has been carried out successfully by the modification of our procedure, using acetic anhydride as the solvent.The ether is distilled under reduced pressure with a 50 water bath, leaving.39.5.This solid is dissolved in 3040.
Several organic solvents (tetrahydrofuran, benzene, n -hexane) 7 and particularly acetic anhydride 5, 8 may be used instead of dry ether.
Of 2 hydrochloric acid.
An efficient magnetic stirrer may be substituted.
(0.188.-atom) of activated zinc (Note 6) is added over a 23 minute period.
Filtration and washing should be done as rapidly as possible to minimize exposure of the activated zinc to air.