i've been having this problem extracting loperamide because of the polymer matrix hypomellose.
hydroxypropyl methylcelluose it swells and entrains all the methanol.
so i found this paper instructive.
http://www.aapspharmscitech.org/view.asp?art=pt020208
soon i will have the catalyst and the ammomium formate to try the cth reduction of the chlorine atom on the loperamide molecule.
after that i will try the propyl ester and see if it is any better.
as soon as the formic acid gets here i'll keep you informed.
the general idea of hydrodehalogenation of aromatic chlorocarbons was inspired by this piece of work
Tetrahedron Letters, n00b 26(11) pp. 1381-4, 1985; M. K. Anwer & A. F. Spatola; Applications of Amm. Formate CTH - IV: A facile method for dehalogenation of aromatic chlorocarbons.
basically chlorobenzene pd/c catalyst methanol solvent and ammonium formate (hydrogen donor)
is stirred 30 minutes to get quantitative yeilds.
and yes the tertiary benzylic alcohol is unaffected by this.
hydroxypropyl methylcelluose it swells and entrains all the methanol.
so i found this paper instructive.
http://www.aapspharmscitech.org/view.asp?art=pt020208
soon i will have the catalyst and the ammomium formate to try the cth reduction of the chlorine atom on the loperamide molecule.
after that i will try the propyl ester and see if it is any better.
as soon as the formic acid gets here i'll keep you informed.
the general idea of hydrodehalogenation of aromatic chlorocarbons was inspired by this piece of work
Tetrahedron Letters, n00b 26(11) pp. 1381-4, 1985; M. K. Anwer & A. F. Spatola; Applications of Amm. Formate CTH - IV: A facile method for dehalogenation of aromatic chlorocarbons.
basically chlorobenzene pd/c catalyst methanol solvent and ammonium formate (hydrogen donor)
is stirred 30 minutes to get quantitative yeilds.
and yes the tertiary benzylic alcohol is unaffected by this.