반응 #71865

반응 방정식

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

수율 87.7%

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

수율 87.7%

용매

water

반응 조건

후처리

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

실험 절차

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%).

출처