Patent ID: 6593473
Filing Date: 2003-07-15
Classification: C07D

Abstract:
A process for the preparation of granular N-alkylammoniumacetonitrile salts of the formula IR2R3N+R1â€”CR4R5â€”CN Yâˆ’â€ƒâ€ƒ(I) whereinR1 is a C1- to C24 -alkyl group, which can be interrupted by nonadjacent oxygen atoms or can carry additional hydroxyl groups, a C4- to C24-cycloalkyl group, a C7- to C24-alkaryl group or a group of the formula â€”CR4R5â€”CN, R2 and R3 in each case independently of one another have the meaning of R1 or together are a saturated 4- to 9-membered ring having at least one carbon atom and at least one other heteroatom from the group consisting of oxygen, sulfur and nitrogen, R4 and R5 in each case independently of one another are hydrogen, C1- to C24-alkyl groups, which can be interrupted by nonadjacent oxygen atoms or can additionally carry hydroxyl groups, C4- to C24-cycloalkyl groups or C7- to C24-alkaryl groups, and Yâˆ’ is a sulfate or hydrogensulfate anion in the corresponding stoichiometric amount, from an aqueous solution of the compound of the formula II R2R3N+R1â€”CR4R5â€”CN R6Oâ€”SO2â€”Oâˆ’â€ƒâ€ƒ(II) wherein R1 to R5 are as defined above and R6 is C1- to C4-alkyl, comprising:(a) evaporating said aqueous solution at a temperature ranging from 80Â° C. to 250Â° C. and a pressure ranging from 10 mbar to 2 bar to give a melt having a residual water content of at most 20% by weight, (b) allowing the melt to solidify, where, during or following the evaporation, customary carrier materials and/or auxiliaries can be added, and (c) converting the solidified compound I obtained from (b) into the desired granular form, wherein hydrolysis of the counterion R6Oâ€”SO2Oâˆ’ to Yâˆ’ takes place thermally and without the addition of an acid.