反应详情

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.3 g--see Preparation 8), 4-sulphamoylphenethyl chloride (0.23 g--see J. Pharm. Pharmacol., 16, 541, (1964)), sodium bicarbonate (0.4 g) and acetonitrile (10 ml) was heated under reflux for 2 hours. A further portion of sodium bicarbonate (1 g) was added followed by potassium iodide (0.2 g) and the mixture was heated under reflux for 2 hours. On cooling to room temperature, water (60 ml) was added and the mixture was extracted with dichloromethane (3×50 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a glass which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a colourless foam, yield, 0.11 g.

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. temperaturethe mixture was heated
4. temperatureunder reflux for 2 hours
5. extractionthe mixture was extracted with dichloromethane (3×50 ml)
6. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customto give a glass which
9. customwas purified by column chromatography on silica eluting with dichloromethane
10. additioncontaining methanol (0% up to 10%)
11. concentrationconcentrated in vacuo