Method for preparing 5-carbamoyl-5H-dibenz[b,f]azepine

Details Method for preparing 5-carbamoyl-5H-dibenz[b,f]azepine Method for preparing 5-carbamoyl-5H-dibenz[b,f]azepine

1991-07-01

1993-02-09

Bond, Robert T.

Organic compounds -- part of the class 532-570 series

Organic compounds

Unsubstituted hydrocarbyl chain between the ring and the -c-...

C07D22320

Patent

active

051854430

ABSTRACT:
A process for producing carbamazepine ##STR1## by (i) optionally purifying a solution of CCDA ##STR2## in an anhydrous, aromatic solvent; (ii) if required distilling off water in the solution; (iii) diluting the water-free solution with an additional amount of the anhydrous, aromatic solvent; (iv) in a reactor aminating the diluted solution at from about 70.degree. C. to about 105.degree. C. with an excess of ammonia to form a mixture of carbamazepine and ammonium chloride; (v) before completion of the amination introducing from about 10% to about 40% wt based on the solution of water into the mixture to obtain a crystal structure which facilitates stirring and thus completion of the amination; (vi) completing the amination by continuing the introduction of ammonia gas until the substantially complete conversion of CCDA to carbamazepine; (vii) separating crystalline carbamazepine/ammonium chloride mixture; (viii) dissolving ammonium chloride in the mixture with water; and (ix) recovering the crystalline carbamazepine which remained solid.

REFERENCES:
patent: 2762796 (1956-09-01), Morel et al.

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