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3-[(Z)-4-Chloro-phenylimino]-5-{(Z)-6-[5-[(Z)-4-chloro-phenylimino]-4,5-dihydro-[1,2,4]triazol-(3Z)-ylideneamino]-hexylimino}-4,5-dihydro-3H-[1,2,4]triazole[ No CAS ]
Referential Example 1 19.1 g of hexamethylene.bis-dicyandiamide obtained in Example 1 (i)(ii) and 25.0 g of p-chloroaniline hydrochloride are dissolved in 180 ml of 2-ethoxyethanol with warming, then the mixture is refluxed for 3 hours with stirring. Next, the reaction mixture is cooled and crystal is filtered and dried to yield 39.7 g of chlorhexidine hydrochloride, m.p. 260-262 C. (yield 90.3%).
89.6%
Referential Example 2 In the same manner as in Referential Example 1, hexamethylene.bis-dicyandiamide obtained in Example 2 is reacted with p-chloroaniline hydrochloride to yield chlorhexidine hydrochloride, m.p. 260-262 C. (yield 89.6%).
89.3%
Referential Example 3 Using hexamethylene.bis-dicyandiamide obtained in Example 3 (i)(ii) and employing the procedure outlined in Referential Example 1, the reaction is carried out to yield chlorhexidine hydrochloride, m.p. 260-262 C. (yield 89.3%).
87.5%
Referential Example 6 Using hexamethylene.bis-dicyandiamide obtained in Example 6 (i)(ii) and employing the procedure outlined in Referential Example 1, the reaction is carried out to yield chlorhexidine hydrochloride, m.p. 260-262 C. (yield 87.5%).
85.4%
Referential Example 5 Using hexamethylene.bis-dicyandiamide obtained in Example 5 (i)(ii) and employing the procedure outlined in Referential Example 1, the reaction is carried out to yield chlorhexidine hydrochloride, m.p. 260-262 C. (yield 85.4%).
82.1%
Referential Example 4 21.3 g of hexamethylene.bis-dicyandiamide obtained in Example 4 (i)(ii) and 27.9 g of p-chloraniline hydrochloride are dissolved in 200 ml of 2-ethoxyethanol with warming, then the mixture is refluxed for 3 hours with stirring. Next, the reaction mixture is cooled and crystal is filtered and dried to yield 40.4 g of chlorhexidine hydrochloride, m.p. 260-262 C. (yield 82.1%).
Referential Example 7 In the same manner as in Referential Example 1, hexamethylene.bis-dicyandiamide (V) obtained in Example 7 is reacted to yield chlorhexidine hydrochloride (m.p. 260-262 C.).
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