反应详情

A solution of INT 58 (206 mg, 0.431 mmol) in CH2Cl2 (5 mL) was treated with HCl (4 M in dioxane, 0.43 mL, 1.726 mmol) and stirred at room temperature overnight. The mixture contained some starting material, so another portion of HCl (4 M in dioxane, 0.50 ml, 2.00 mmol) was added and stirring continued for 4 hours. Excess of HCl gas was removed by a stream of argon. The mixture was neutralized with 10% sodium bicarbonate solution then treated with 10% ammonium chloride solution and extracted first with CH2Cl2 then with EtOAc. The combined organic layers were dried over sodium sulfate, filtered and concentrated. The title compound was purified by preparative UPLC (H2O/CH3CN).

1. stirringstirring
2. waitcontinued for 4 hours
3. customExcess of HCl gas was removed by a stream of argon
4. additionthen treated with 10% ammonium chloride solution
5. extractionextracted first with CH2Cl2
6. dry with materialThe combined organic layers were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe title compound was purified by preparative UPLC (H2O/CH3CN)