Large-scale Mda Synthesis Form Piperonal

Large-scale MDA from piperonal ------------------------------------------------------------------------------STEP 1 (Makin' da nitroalkene) Dissolve 1000 g of piperonal into 500 g of nitroethane containing  g of c!clohe"!la#ine and let the #i" stand for a$o%t & eeks Then cr%sh !o%r 'chicken !ello' nitroalkene cake and ash it ith a$o%t * liters of free+er cold Me, Spread to dr! ./ED 23,4T 1000 T, 1100 g STEP * (ed%cin' da a$ove #entionned st%fff) st%fff) To *00 g of i2l6 dissolved in 10  of ice cold anh!dro%s T7 add dropise ith cooling 5*0 g of ra MDP-*-8P (straight fro# the previo%s step) dissolved in 5  of T7 The addition sho%ld take $eteen 1 to & ho%rs ith proper cooling of the reaction #i" Stir at roo# te#perat%re for & ho%rs (8, E749:) Then add to the #i" containing the no red%ced co#po%nd 1000 #l of /P2 to deco#pose the resid%al i2l6 folloed $! 600 #l of 15; a<%eo%s 8a, 7ilter the solids (2l = i salts) fro# the reaction #i" and >2E74. ash the filter cake %sing the re#aining 5  of T7 fro# !o%r *0  dr%# Evaporate the solvents and cr!stali+e the free $ase '? la Sh%lgin' to get a$o%t 00 g ($eteen 500 to @00 g) of the prod%ct >l ./ED a$o%t 00 g of hite fl%ff! st%ff --------------------------------------------