反应详情

To 3e (120 mg, 0.26 mmol) in CH2Cl2 (3 mL) was added iPr2NEt (0.12 mL, 0.66 mmol), followed by chloroacetyl chloride (0.03 mL, 0.40 mmol), and the reaction was stirred at room temperature. Once complete, the reaction was diluted with water, and the aqueous layer was extracted with CH2Cl2. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the residue was dissolved in C2H4Cl2. iPr2NEt (0.12 mL, 0.66 mol) was added, and the reaction was sealed and heated to 80° C. overnight. After cooling to room temperature, the reaction was concentrated and purified by preparative HPLC to give the desired product.

1. extractionthe aqueous layer was extracted with CH2Cl2
2. dry with materialThe combined organic layers were dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionthe residue was dissolved in C2H4Cl2
6. customthe reaction was sealed
7. temperatureheated to 80° C. overnight
8. temperatureAfter cooling to room temperature
9. concentrationthe reaction was concentrated
10. custompurified by preparative HPLC