4-Bromophenol → 4-(4-Bromophenoxy)butanoic acid

4-Bromo-phenol (172 g, 1 mol), 4-bromo-butyric acid ethyl ester (212 g, 1.1 mol) and K2CO3 (250 g, 1.8 mol) was dissolved in DMF (1000 mL), the mixture was stirred at room temperature overnight. the solvent was removed and water was added to the residue, the mixture was extracted with ethyl acetate, the organic layer was washed with brine, and dried over Na2SO4 the solvent was removed, to the residue was added NaOH (3M, 1000 mol) and CH3OH (600 mL), the mixture was stirred at 70 for 30 minutes and concentrated, the residue was dissolved in H2O and the mixture was washed with diethylether, the aqueous layer was acidified with HCl, and the mixture was extracted with ethyl acetate, the organic layer was washed with brine, dried over Na2SO4, concentrated to give crude 4-(4-bromophenoxy)butanoic acid (239 g, 98%).

1. customthe solvent was removed
2. additionwater was added to the residue
3. extractionthe mixture was extracted with ethyl acetate
4. washthe organic layer was washed with brine
5. dry with materialdried over Na2SO4 the solvent
6. customwas removed, to the residue
7. stirringthe mixture was stirred at 70 for 30 minutes
8. concentrationconcentrated
9. dissolutionthe residue was dissolved in H2O
10. washthe mixture was washed with diethylether
11. extractionthe mixture was extracted with ethyl acetate
12. washthe organic layer was washed with brine
13. dry with materialdried over Na2SO4
14. concentrationconcentrated

ORDレコード

ord-778a54ad4bbe49beb8f59bf9ed31a94e

出典データセット

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08921359B2