Реакция #71865

Уравнение реакции

DMF

methyl 3-[(7-nitro-2,3-dihydro-4H-1,4-benzoxazin-4-yl)methyl]benzoate

Methyl 3-[(7-nitro-2,3-dihydro-4H-1,4-benzoxazin-4-yl)methyl]benzoate

→

crude title compound

Выход 87.7%

Methyl 3-[(7-amino-2,3-dihydro-4H-1,4-benzoxazin-4-yl)methyl]benzoate

Выход 87.7%

Растворители

water

Условия реакции

Обработка

1. 1
   ФильтрацияThe insoluble matter was filtered off
2. 2
   workup.ADDITIONethyl acetate was added to the mother liquor
3. 3
   Промывкаthe organic layer was washed with water and brine
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   КонцентрированиеConcentration under reduced pressure

Методика

DMF (5 mL), water (5 mL), zinc (0.7 g, 10.7 mmol) and iron trichloride hexahydrate (0.12 g, 0.4 mmol) were added to methyl 3-[(7-nitro-2,3-dihydro-4H-1,4-benzoxazin-4-yl)methyl]benzoate obtained in Example (100a) (0.35 g, 1.07 mmol), and the mixture was stirred at 100° C. for 50 minutes. The insoluble matter was filtered off and ethyl acetate was added to the mother liquor, and the organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. Concentration under reduced pressure gave 0.28 g of the crude title compound as a brown oily substance (88%).

Источник