反应详情

The product of step (a) (2 g; 6.3291 mmole) was dissolved in ethanol and hydrogen chloride was bubbled through the solution. When the heat of soluation subsided, the solution was heated to reflux on a steambath for 2 hours. The mixture was cooled, treated with water and concentrated, followed by basification with NH3 solution (pH about 6). The solution was extracted into chloroform and this was washed with water, dried and evaporated to give a brown solid (1.6 g, 76%). NMR and mass spectra were consistent with required structure.

1. customhydrogen chloride was bubbled through the solution
2. temperatureWhen the heat of soluation
3. temperaturethe solution was heated
4. temperatureto reflux on a steambath for 2 hours
5. temperatureThe mixture was cooled
6. additiontreated with water
7. concentrationconcentrated
8. extractionThe solution was extracted into chloroform
9. washthis was washed with water
10. customdried
11. customevaporated