反应详情

To a solution of the product of Example 39-5 (407 g, 0.754 mol) in dichloromethane (550 mL) was added 4 M HCl in dioxane (760 mL, 3.04 mol) and the solution was mixed at RT for 3.5 h. The reaction was quenched by addition of ethyl acetate (1.5 L) and pH 7 phosphate buffer (1.7 L) and the layers were separated. The aqueous layer was back-extracted with ethyl acetate (400 mL) and the combined organic layers were concentrated and chased with ethanol to a final volume of approximately 2500 mL. The product precipitated and was isolated by filtration and dried to give the title compound (309.7 g, 93.4%).

1. additionthe solution was mixed at RT for 3.5 h
2. customThe reaction was quenched by addition of ethyl acetate (1.5 L) and pH 7 phosphate buffer (1.7 L)
3. customthe layers were separated
4. extractionThe aqueous layer was back-extracted with ethyl acetate (400 mL)
5. concentrationthe combined organic layers were concentrated
6. customThe product precipitated
7. customwas isolated by filtration
8. customdried