反应详情

Following the procedure of Example 5, a stirred solution of 1.38 g. of 2-([2-(dimethylaminomethyl)-5-methyl-4-thiazolyl]methylthio)ethylamine in 10 ml. of methanol was treated with N-methyl-1-methylthio-2-nitroethyleneamine. The reaction mixture was kept at room temperature overnight by which time all solids had dissolved. Thin layer chromatography over silica using a 10:10:1 ethyl acetate-methanol-ammonium hydroxide solvent system indicated substantially a single product. The reaction mixture was concentrated by evaporation of the methanol and the resulting gummy yellow residue was triturated with several portions of cold ether, thus providing an off-white gum. Repeated tritration with cold 1,2-dimethoxyethane yielded N-2-([2-(dimethylaminomethyl)-5-methyl-4-thiazolyl]methylthio)ethyl-N'-methyl-2-nitro-1,1-ethenediamine formed in the above reaction melting at about 104°-106° C.

1. dissolutionall solids had dissolved
2. concentrationThe reaction mixture was concentrated by evaporation of the methanol
3. customthe resulting gummy yellow residue was triturated with several portions of cold ether
4. customthus providing an off-white gum