反应详情

温度

0 °C

A solution of 3-phenylisocarbostyril (0.1 g) in N,N-dimethylformamide (2 ml) was cooled to 0° C. under an inert atmosphere. Sodium hydride (0.019 g) was added and the resulting mixture stirred at 0° C. for 5 minutes. 3,4-Dimethoxybenzenesulphonylchloride (0.107 g) was added over a 3 minute period, with continued stirring at 0° C. for a further 15 minutes. The reaction mixture was warmed to room temperature and stirred for 24 hours. The DMF was evaporated under high vacuum and the residue partitioned between ethyl acetate (2×12 ml) and water (12 ml). The combined organic phases were dried over magnesium sulphate and concentrated in vacuo to yield a yellow oil. Purification using column chromatography eluting with 50% ethyl acetate in hexane yielded an oil which was crystallized from ethyl acetate/hexane to furnish the title compound as white crystals (0.089 g).

1. stirringwith continued stirring at 0° C. for a further 15 minutes
2. temperatureThe reaction mixture was warmed to room temperature
3. stirringstirred for 24 hours
4. customThe DMF was evaporated under high vacuum
5. customthe residue partitioned between ethyl acetate (2×12 ml) and water (12 ml)
6. dry with materialThe combined organic phases were dried over magnesium sulphate
7. concentrationconcentrated in vacuo
8. customto yield a yellow oil
9. customPurification
10. washeluting with 50% ethyl acetate in hexane
11. customyielded an oil which
12. customwas crystallized from ethyl acetate/hexane