反应详情

温度

50 °C

The product from example 18 step (ii) (1.44 g) was dissolved in dry N,N-dimethylformamide (20 ml) and treated cautiously with sodium hydride (60% dispersion by wt, 0.5 g) under nitrogen. After 10 min 1-(2-chloroethyl)pyrrolidine hydrochloride (0.8 g) was added and the whole heated at 50° C. for 16 h. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was collected, dried over magnesium sulphate and solvent evaporated under reduced pressure. Purification was by flash chromatography eluting with 9:1 dichloromethane/methanol. The product obtained was dissolved in acetic acid (10 ml) and heated at 100° C. for 2 h. The solvent was removed under reduced pressure. Purification was by flash chromatography eluting with dichloromethane/methanol mixtures to give the subtitle product as pale yellow foam.

1. customThe reaction mixture was partitioned between water and ethyl acetate
2. customThe organic layer was collected
3. dry with materialdried over magnesium sulphate and solvent
4. customevaporated under reduced pressure
5. customPurification
6. washeluting with 9:1 dichloromethane/methanol
7. customThe product obtained
8. temperatureheated at 100° C. for 2 h
9. customThe solvent was removed under reduced pressure
10. customPurification
11. washeluting with dichloromethane/methanol