反应详情

A mixture of 1-[[[5-[(dimethylamino)methyl]-2-furanyl]-methyl]thio]methanimidamide maleate (1:2) (2.23 g), N-(2-chloroethyl)-N'-methyl-2-nitro-1,1-ethenediamine (0.9 g) and potassium carbonate (3.46 g) in water (10 ml) and tetrahydrofuran (10 ml) was stirred under nitrogen at room temperature for 5 days. The suspension was evaporated in vacuo; the residue suspended in water (50 ml) and extracted with ether (2×40 ml). The aqueous fraction was evaporated in vacuo and magnesium sulphate and tetrahhydrofuran (100 ml) added. After 18 hours, the mixture was filtered and the filtrate evaporated to give a semi-solid which was chromatographed (silica/methanol). The appropriate eluate was evaporated in vacuo to give the title compound (0.3 g), which had an n.m.r. identical to that of the product according to Example 1 above.

1. customThe suspension was evaporated in vacuo
2. extractionextracted with ether (2×40 ml)
3. customThe aqueous fraction was evaporated in vacuo and magnesium sulphate and tetrahhydrofuran (100 ml)
4. additionadded
5. waitAfter 18 hours
6. filtrationthe mixture was filtered
7. customthe filtrate evaporated
8. customto give a semi-solid which
9. customwas chromatographed (silica/methanol)
10. customThe appropriate eluate was evaporated in vacuo