반응 #94852
ord-cdd4b4daba06472ea32bc0b00c8c0aaf
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후처리
- 1기타The residue, obtained on evaporation of the reaction mixture
- 2세척Elution of the appropriate region of the chromatogram
- 3기타with hot ethanol and evaporation of the solvent
- 4기타gave a glass-like material
실험 절차
To a solution of 2-guanidino-4-(3-aminocyclohexyl)thiazole (0.3 g.) in ethanol (30 ml.) was added 2-methyl-1-nitroisothiourea (0.2 g.) and the mixture allowed to stand overnight at room temperature. The residue, obtained on evaporation of the reaction mixture, was subjected to preparative thin layer chromatography on silica gel GF plates (Uniplate, Analtech Inc. Delaware, USA) using chloroform:methanol:ammonia (s.g. 0.88) 80:20:0.5 v/v/v for development. Elution of the appropriate region of the chromatogram with hot ethanol and evaporation of the solvent gave a glass-like material. This was dissolved in a small volume of ethanol and the solution treated with a solution of maleic acid in acetone. The resulting solution was diluted with ether to give 2-guanidino-4-[3-(2-nitroguanidino)cyclohexyl] thiazole maleate hemihydrate (0.12 g.) which was obtained as an amorphous solid. The n.m.r. spectrum in d6 dimethylsulphoxide included resonances at 1.2 (brm), 1.8 (brm), 2.7 (m) 3.5(m) 6.11(s-maleic acid olefinic protons), 6.9(s), 8.05 (m) and 8.14 (brs).