first of all, hi bee's
I have floated in over the last few (3) years thx to you all
swim is interested in forming 2c-i ala shulgin from
"N-(2-(2,5-dimethoxyphenyl)ethyl)phthalimide"
but alas swim has no idea of what conc acetic acid or any idea
on what conc hydrazine hydrate to use either.
here is what shulgin did
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To a solution of 12.9 g N-(2-(2,5-dimethoxyphenyl)ethyl)phthalimide in 130 mL warm (35 deg C) acetic acid which was
being vigorously stirred, there was added a solution of 10 g iodine monochloride in 40 mL acetic acid. This was
stirred for 1 h, while being held at about 30 deg C. The reaction mixture was poured into 1500 mL H2O and extracted
with 4x75 mL CH2Cl2. The extracts were pooled, washed once with 150 mL H2O containing 2.0 g sodium dithionite, and
the solvent removed under vacuum to give 16.2 g of N-(2-(2,5-dimethoxy-4-iodophenyl)ethyl)phthalimide as yellow amber
solids with a mp of 133-141 deg C. This mp was improved by recrystallization from 75 mL CH3CN, yielding 12.2 g of a
pale yellow solid with mp 149-151 deg C. A small sample from a large quantity of IPA gives a white product melting at
155.5-157 deg C.
A solution of 12.2 g N-(2-(2,5-dimethoxy-4-iodophenyl)ethyl)phthalimide in 150 mL hot IPA was treated with 6.0 mL
of hydrazine hydrate, and the clear solution was heated on the steam bath. After a few minutes there was the generation
of a white cottage cheese-like solid (1,4-dihydroxyphthalizine). The heating was continued for several additional h,
the reaction mixture cooled, and the solids removed by filtration. These were washed with 2x10 mL EtOH, and the pooled
filtrate and washes stripped of solvent under vacuum giving a residue which, when treated with aqueous hydrochloric acid,
gave 3.43 g of voluminous white crystals. This, after recrystallization from 2 weights of H2O, filtering, washing first
with IPA and then with Et2O, and air drying, gave 2.16 g 2,5-dimethoxy-4-iodophenethylamine hydrochloride (2C-I) as a
white microcrystalline solid, with a mp of 246-247 deg C. Anal. (C10H15ClINO2) C,H,N.
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swim has succeded creating a few amphetamines and wishes to try something a little more
interesting with a modest chem background (alas no formal organic chem training) and
an optimistic heart i throw this help line out.
this is my first post and yes i have utfse
any help both on the chems and on post structure thx