반응 #94862
ord-1b8fe65dc4fe4f8abfe947e48e2116da
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반응물
시약
반응 조건
후처리
- 1기타The residue obtained by evaporation of the solvent
- 2기타was partitioned between ethyl acetate (100 ml.) and water (20 ml.) The organic layer
- 3기타was isolated
- 4세척washed with water (20 ml)
- 5건조dried (magnesium sulphate)
- 6기타evaporated
- 7기타The appropriate zone of the chromatogram was isolated
- 8추출extracted with hot ethanol/chloroform 50:50 v/v (200 ml.)
- 9기타the residue obtained on evaporation of the solvents
- 10기타followed by a further amount of ether until precipitation
- 11세척The white powder precipitate (0.2 g.) was washed with ether
실험 절차
To a solution of 2-guanidino-4-{3-[3-cyano-2-(2-aminoethyl)guanidino]cyclohexyl}thiazole (0.5 g.) in methanol (30 ml.) was added o-chlorobenzoyl chloride (0.4 g.) and the mixture allowed to stand at room temperature for 16 hours. The residue obtained by evaporation of the solvent was partitioned between ethyl acetate (100 ml.) and water (20 ml.) The organic layer was isolated, washed with water (20 ml), dried (magnesium sulphate) and evaporated. The residue was subjected to preparative thin layer chromatography on Merck 60 F-254 plates using chloroform/methanol/aqueous ammonia (s.g. 0.88) 80:20:0.1 v/v/v for development. The appropriate zone of the chromatogram was isolated and extracted with hot ethanol/chloroform 50:50 v/v (200 ml.) and the residue obtained on evaporation of the solvents was dissolved in methanol. To this solution was added an excess of maleic acid in ether followed by a further amount of ether until precipitation began. The white powder precipitate (0.2 g.) was washed with ether to give 2-guanidino-4-{ 3-[3-cyano-2-(2-(2-chlorobenzoylamino)ethyl)guanidino]cyclohexyl}thiazole hydrogen maleate, m.p. 158°-165° (decomp.).