反应详情

温度

90 °C

A mixture of the product of step (iv) (250 mg, 0.61 mmol), K2CO3 (250 mg, 1.8 mmol), 3-methoxypropylamine (82 mg, 0.92 mmol) in MeCN (20 mL, Aldrich, HPLC grade) was stirred at 90° C. under N2 atmosphere overnight. The reaction mixture was cooled to room temperature and filtered. The filtrate was concentrated in vacuo and the residue subjected to prep-HPLC for purification, the eluents were concentrated and 1N NaOH solution added into the residue to control the pH=8˜9. The mixture was extracted with DCM three times. The combined extracts was dried over anhydrous sodium sulphate, filtered, concentrated in vacuo, which afforded the title compound (yellow solid, 158 mg)

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. concentrationThe filtrate was concentrated in vacuo
4. customprep-HPLC for purification
5. concentrationthe eluents were concentrated
6. addition1N NaOH solution added into the residue
7. extractionThe mixture was extracted with DCM three times
8. dry with materialThe combined extracts was dried over anhydrous sodium sulphate
9. filtrationfiltered
10. concentrationconcentrated in vacuo, which