反应详情

温度

50 °C

14A (300 mg, 0.889 mmol) was treated with acetonitrile (2 mL) and THF (0.5 mL). This clear solution was treated with N,N-dimethylformamide dimethylacetal (0.30 mL, 2.22 mmol) and the reaction mixture was stirred at 50° C. for 45 min. The mixture was treated with 2-methoxyethanamine (0.230 mL, 2.67 mmol) resulting in a yellow clear solution. Acetic acid (0.5 mL, 8.73 mmol) was added, and the reaction was stirred at 90° C. overnight. The reaction was diluted with water and extracted with 25% MeOH in dichloromethane (3×). The combined organic extracts were washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. The residue was purified by Isco silica column (12 g), (gradient elution with methanol-dichloromethane over 12 min.) Concentration of the appropriate fractions provided 14B (300 mg, 0.742 mmol, 83% yield) as a pale yellow oil. MS (ES): m/z=405.2 [M+H]+.

1. customresulting in a yellow clear solution
2. stirringthe reaction was stirred at 90° C. overnight
3. extractionextracted with 25% MeOH in dichloromethane (3×)
4. washThe combined organic extracts were washed with brine
5. dry with materialdried over anhydrous sodium sulphate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by Isco silica column (12 g), (gradient elution with methanol-dichloromethane over 12 min.) Concentration of the appropriate fractions