反应详情

A mixture of 2.0 g. (8 mmoles) of 2-(2-ethylamino-4-pyridyl)-2,2-diethoxyethylamine, 1.0 g. (8.3 mmoles) of ethyl acetimidate hydrochloride and 30 ml. of absolute ethanol was heated at reflux for 1.3 hours. The mixture was concentrated, and the residue taken up in 10 ml. of concentrated hydrochloric acid. The acid solution was heated on a steam bath for one hour and the cooled reaction made basic by the addition of solid potassium carbonate. The product was extracted with chloroform (4×15 ml.) and the combined extracts dried and concentrated to give 1.1 g. of crude product. The product was chromatographed over 35 g. of silica gel using chloroform-methanol (19:1, v:v) as the eluent to give 510 mg. (30%), m.p. 214°-216° C.

1. additionA mixture of 2.0 g
2. temperatureat reflux for 1.3 hours
3. concentrationThe mixture was concentrated
4. temperatureThe acid solution was heated on a steam bath for one hour
5. customthe cooled reaction
6. extractionThe product was extracted with chloroform (4×15 ml.)
7. customthe combined extracts dried
8. concentrationconcentrated
9. customto give 1.1 g
10. customThe product was chromatographed over 35 g
11. customto give 510 mg