反应详情

A mixture of 4-(6-aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole trihydrochloride (1.5 g), triethylamine (1.8 ml), (furfurylthio)acetic acid (0.8 g), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (1.0 g) in N,N-dimethylformamide (15 ml) was stirred at ambient temperature for 18 hours. The mixture was added to a mixture of ethyl acetate and water and the separated organic layer was dried over magnesium sulfate. Evaporation of the solvent gave a residue, which was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (9:1, V/V). The eluted fractions containing the desired product were collected and evaporated in vacuo. The residue was recrystallized from a mixture of methanol, dioxane and diisopropyl ether to give 2-(diaminomethyleneamino)-4-[6-(furfurylthio)acetylaminomethylpyridin-2-yl)thiazole (0.73 g).

1. dry with materialthe separated organic layer was dried over magnesium sulfate
2. customEvaporation of the solvent
3. customgave a residue, which
4. customwas purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (9:1, V/V)
5. additionThe eluted fractions containing the desired product
6. customwere collected
7. customevaporated in vacuo
8. customThe residue was recrystallized from a mixture of methanol, dioxane and diisopropyl ether