反应详情

The product from Stage (b) (3.1 g) in dry tetrahydrofuran (10 ml) was added dropwise to stirred, cooled (5° C.) methanesulfonamide sodium salt (2.8 g) in dry tetrahydrofuran (25 ml). Stirring was continued until most solid had dissolved (2 hours) and the reaction mixture was allowed to stand at room temperature overnight. The solvent was then evaporated off under vacuum and the residue was treated with ether. The precipitated solid was taken up in aqueous potassium bicarbonate, the ether solution extracted again with bicarbonate and then with water. The combined aqueous phases were washed with ether, fresh ether was then added and the whole was acidified to pH=1 with hydrochloric acid as quickly as possible with stirring. The ether solution was separated, and the aqueous phase was extracted twice more. The combined ether solutions were washed with water (5 times), dried over magnesium sulfate and evaporated under vacuum to give 2.3 g of the desired product. Washing with a small volume of diisopropyl ether gave 1.95 g of pure product as a viscous liquid.

1. stirringStirring
2. dissolutionhad dissolved (2 hours)
3. customThe solvent was then evaporated off under vacuum
4. additionthe residue was treated with ether
5. extractionthe ether solution extracted again with bicarbonate
6. washThe combined aqueous phases were washed with ether, fresh ether
7. additionwas then added
8. stirringwith stirring
9. customThe ether solution was separated
10. extractionthe aqueous phase was extracted twice more
11. washThe combined ether solutions were washed with water (5 times)
12. dry with materialdried over magnesium sulfate
13. customevaporated under vacuum