반응 #63092

반응 방정식

2-[2-(2,2,2-trifluoroethyl)guanidino]-4-[4-(3-[2-aminophenyl]thioureido)butyl]thiazole

triethylamine

→

2-[4-(2-[2-(2,2,2-trifluoroethyl)guanidino]thiazol-4-yl)butylamino]benzimidazole

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타Hydrogen sulphide gas was then bubbled through the reaction mixture until no more solid
2. 2
   기타precipitated
3. 3
   여과The reaction mixture was filtered through a pad of diatomaceous earth
4. 4
   기타the filtrate evaporated to dryness in vacuo
5. 5
   기타The residue was purified by low pressure liquid chromatography

실험 절차

A mixture of 2-[2-(2,2,2-trifluoroethyl)guanidino]-4-[4-(3-[2-aminophenyl]thioureido)butyl]thiazole (0.45 g.), silver nitrate (0.34 g.) and triethylamine (0.28 ml.) in dimethylformamide (3 ml.) was stirred vigorously at ambient temperature overnight. Hydrogen sulphide gas was then bubbled through the reaction mixture until no more solid precipitated. The reaction mixture was filtered through a pad of diatomaceous earth and the filtrate evaporated to dryness in vacuo. The residue was purified by low pressure liquid chromatography using chloroform/methanol/ammonia, 9:1:0.1 v/v/v as eluant to give 2-[4-(2-[2-(2,2,2-trifluoroethyl)guanidino]thiazol-4-yl)butylamino]benzimidazole which was converted to the hydrogen maleate salt (0.25 g.), m.p. 183°-186°.

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