반응 #92686

반응 방정식

methyl 5-[(2-fluorobenzyl)oxy]-6-nitronicotinate

ethanol

water

ammonium chloride

→

methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate

수율 99.8%

용매

THF

반응 조건

후처리

1. 1
   온도by heating
2. 2
   온도to reflux for 2 hours
3. 3
   기타After leaving
4. 4
   여과the reaction mixture was filtered over Celite
5. 5
   workup.ADDITIONto the filtrate were added a saturated aqueous sodium hydrogen carbonate solution and chloroform
6. 6
   기타a layer separation operation
7. 7
   건조The organic layer was dried over anhydrous sodium sulfate
8. 8
   기타the solvent was evaporated under reduced pressure

실험 절차

To a solution of 2.5 g of methyl 5-[(2-fluorobenzyl)oxy]-6-nitronicotinate in 25 ml of THF were added 50 ml of ethanol, 25 ml of water, 218 mg of ammonium chloride, and 1.37 g of iron, followed by heating to reflux for 2 hours. After leaving to be cooled at room temperature, the reaction mixture was filtered over Celite, and to the filtrate were added a saturated aqueous sodium hydrogen carbonate solution and chloroform to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure to obtain 2.25 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate.

출처