反応 #71865

反応方程式

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

収率 87.7%

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

収率 87.7%

溶媒

water

反応条件

後処理

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

実験手順

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%).

出典