反应 #71865

反应方程式

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

收率 87.7%

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

收率 87.7%

溶剂

water

反应条件

后处理

1. 1
   过滤The insoluble matter was filtered off
2. 2
   workup.ADDITIONethyl acetate was added to the mother liquor
3. 3
   洗涤the organic layer was washed with water and brine
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   浓缩Concentration under reduced pressure

实验过程

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%).

来源