반응 #653278

반응 방정식

methyl 7-(4-fluorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate

THF

sodium hydroxide

→

7-(4-fluorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid

수율 86.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타Under reduced pressure, the solvent was removed
2. 2
   workup.ADDITIONthe residue was diluted with water (100 ml)
3. 3
   추출the mixture was extracted with ethyl acetate (100 ml)
4. 4
   건조The organic layer was dried with anhydrous magnesium sulfate
5. 5
   기타the solvent was removed under reduced pressure
6. 6
   기타The residue was crystallized
7. 7
   세척washed with hexane

실험 절차

To methyl 7-(4-fluorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (0.27 g) were added THF (5.0 ml), ethanol (10.0 ml) and 2N sodium hydroxide solution (1.0 ml), and the mixture was stirred at room temperature for 19 hours. Under reduced pressure, the solvent was removed, and the residue was diluted with water (100 ml). The aqueous layer was made acidic with hydrochloric acid, and the mixture was extracted with ethyl acetate (100 ml). The organic layer was dried with anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was crystallized and washed with hexane to give 7-(4-fluorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (0.22 g, 86%) as white crystals.

출처