反应详情

2.22 g (14 mmol) of 2-chloro-5-nitropyridine and an equimolar equivalent of histamine base (1.56 g) in 10 ml of 2-propanol are brought to reflux for 48 h. The reaction mixture is concentrated to dryness and the solid residue is taken up in water, heated to boiling, cooled and filtered. The filtrate is concentrated to dryness and chromatographed on a column of silica gel which is eluted with a mixture of chloroform and methanol (5, 10 and 20%). The combined pure fractions are evaporated to dryness and the solid residue is crystallized from absolute ethanol to provide the product. M.p.: 162°-163° C.

1. temperatureto reflux for 48 h
2. concentrationThe reaction mixture is concentrated to dryness
3. temperatureheated
4. temperaturecooled
5. filtrationfiltered
6. concentrationThe filtrate is concentrated to dryness
7. customchromatographed on a column of silica gel which
8. washis eluted with a mixture of chloroform and methanol (5, 10 and 20%)
9. customThe combined pure fractions are evaporated to dryness
10. customthe solid residue is crystallized from absolute ethanol
11. customto provide the product