反应详情

温度

50 °C

Aqueous 3.0 M HCl (12 mL) was added to a solution of the product obtained in Step 1 above (5.00 g, 15.9 mmol) in methanol (200 mL). The reaction mixture was stirred at 50° C. for 5 h and concentrated in vacuo. The residue was dissolved in water (50 mL) and basified with K3PO4. The aqueous phase was extracted with ethyl acetate (5×40 mL), dried (MgSO4), and concentrated in vacuo. This gave 3.08 g (91%) of the title compound as a colorless oil which slowly decomposed upon standing. HRMS m/z calcd for C9H12ClN3O (M)+ 213.0669, found 213.0663.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in water (50 mL)
3. extractionThe aqueous phase was extracted with ethyl acetate (5×40 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo