反应详情

温度

68 °C

To a solution of tert-butyl 3-bromo-5-formylbenzoate (119 g, 417 mmol) in dioxane (2.4 L) were added hydroxylamine hydrochloride (44.0 g, 633 mmol) and pyridine (103 mL, 1.27 mol). The reaction mixture was heated to 68° C. After 16 h, the mixture was concentrated. Saturated aqueous amonium chloride was added the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered and concentrated (125.0 g). MS 243 (M-tert-butyl).

1. concentrationthe mixture was concentrated
2. additionSaturated aqueous amonium chloride was added the mixture
3. extractionwas extracted with dichloromethane (3×)
4. washThe combined organic extracts were washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated (125.0 g)