Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he

Details Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he

1988-09-06

1991-08-20

Lee, Mary C.

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

Organic compounds

Amino nitrogen containing

564104, 564303, C07C27702

Patent

active

050416553

ABSTRACT:
An improved method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane from alkali dicyanamide and a hexamethylene diammonium salt in alcoholic solution or suspension. The reaction is carried out in the presence of a limited amount of water and of a catalytic amount of a base, preferably a tertiary amine. The pH of the reaction mixture at the start of the reaction is 8 to 10. After the reaction is over, the reaction mixture is compounded with water at a temperature above 80.degree. C. and the coarse product which crystallizes out is separated from the liquid phase.
Preferably, sodium dicyanamide and hexamethylene diamine dihydrochloride, preferably formed in situ from aqueous 1,6-diaminohexane and aqueous hydrochloric acid, are reacted at pH 9-9.5 in n-butanol in the presence of 0.1 to 20% by wt. water in relation to the solvent including water.
1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane is obtained in a high yield (85-86%) and with great purity (95-97%) and with a considerably improved space-time yield.

REFERENCES:
patent: 2686203 (1954-08-01), Hechenbleikner
patent: 3428576 (1969-02-01), Dickinson et al.
patent: 4217366 (1980-08-01), Kikumoto et al.
patent: 4250109 (1981-02-01), Uchikuga et al.
patent: 4537746 (1985-08-01), Ogunbiyi et al.
patent: 4792570 (1988-12-01), Nelson et al.

Affiliated with

Also associated with

Rating

Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he does not yet have a rating. At this time, there are no reviews or comments for this patent.

If you have personal experience with Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he, we encourage you to share that experience with our LandOfFree.com community. Your opinion is very important and Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) he will most certainly appreciate the feedback.

Rate now

Comments { 0 }

Profile ID: LFUS-PAI-O-1009672