تفاعل #94862
ord-1b8fe65dc4fe4f8abfe947e48e2116da
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1أخرىThe residue obtained by evaporation of the solvent
- 2أخرىwas partitioned between ethyl acetate (100 ml.) and water (20 ml.) The organic layer
- 3أخرىwas isolated
- 4غسيلwashed with water (20 ml)
- 5تجفيفdried (magnesium sulphate)
- 6أخرىevaporated
- 7أخرىThe appropriate zone of the chromatogram was isolated
- 8استخلاصextracted with hot ethanol/chloroform 50:50 v/v (200 ml.)
- 9أخرىthe residue obtained on evaporation of the solvents
- 10أخرىfollowed by a further amount of ether until precipitation
- 11غسيلThe white powder precipitate (0.2 g.) was washed with ether
الإجراء التجريبي
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.).