Abstract:
A process provided for separating an Alpha -amino- omega lactam of the formula:
WHEREIN N IS AN INTEGER FROM 0 TO 12, IN ITS FREE FORM FROM THE REARRANGED MIXTURE OBTAINED BY THE Beckmann rearrangement of an Alpha -aminocycloalkanone oxime of the formula:
WHEREIN N IS AN INTEGER FROM 0 TO 12, WHICH PROCESS COMPRISES THE STEPS OF: CONTACTING THE REARRANGED MIXTURE WITH A SOLVENT SELECTED FROM THE GROUP CONSISTING OF: A. LINEAR AND CYCLIC ETHERS AND POLYETHERS, B. C3 to C8 alcohols in the absence of chloride ions, C. NITRILES CONTAINING TWO OR MORE CARBON ATOMS, D. AROMATICS AND HALOAROMATICS IN THE PRESENCE OF AT LEAST ONE OF SAID (A) OR (B), WHEREIN THE HALO SUBSTITUENT IS CHLORINE OR BROMINE AND IS ATTACHED DIRECTLY TO THE RING, E. CHLOROFORM, F. TRICHLOROETHYLENE IN THE PRESENCE OF AT LEAST ONE OF SAID (A) OR (B), AND G. MIXTURES OF TWO OR MORE OF THE ABOVE, WHILE SIMULTANEOUSLY NEUTRALIZING THE RESULTANT SOLUTION WITH AN EXCESS OF ANHYDROUS AMMONIA BASED ON THE HYDROGEN ION CONCENTRATION IN THE SOLUTION, WHEREBY AN INSOLUBLE AMMONIUM SALT PRECIPITATE IS FORMED; AND SEPARATING A SOLUTION CONTAINING AN Alpha -AMINO- omega -LACTAM IN ITS FREE FORM FROM THE PRECIPITATE.
Abstract:
2-Aminocycloalkanone oximes are produced by reacting, in an oxygen-free environment, hydroxylamine phosphate or hydroxylamine sulfate with anhydrous ammonia; removing the precipitated ammonium salt; adding ammonium chloride to the solution; maintaining the solution within a preselected temperature range while adding 2-chlorocycloalkanone; maintaining the desired temperature until the reaction is complete and isolating the oxime product.
Abstract:
A process of separating an Alpha -amino- omega -lactam having the formula
WHEREIN N IS AN INTEGER FROM 0 TO 12, FROM MIXTURES CONTAINING THE SAME, WHICH PROCESS COMPRISES THE STEPS OF INTRODUCING CARBON DIOXIDE INTO A SOLUTION OF THE Alpha -AMINO- omega -LACTAM IN A SOLVENT SELECTED FROM THE GROUP CONSISTING OF ALIPHATIC KETONES CONTAINING 3 TO 9 CARBON ATOMS, C1 to C4 alkyl esters of C1 to C6 aliphatic carboxylic acids, linear and cyclic ethers and polyethers, chlorobenzene, toluene, chloroform, and mixtures thereof, to form a solid adduct; and separating the solid adduct from the solvent.