Sodium Chloride → HCID 15486834, compound

A mixture of ethyl salicylate (10.0 g, 60.2 mmol), 60% sodium hydride (2.41 g, 60.2 mmol) and N,N-dimethylformamide (150 ml) w as stirred at room temperature for about 1 hour, followed by adding dropwise thereto ethyl 4-bromobutyrate (12.9 g, 66.2 mmol). The reaction mixture was stirred at room temperature for 4.5 hours and then at 65-70° C. for 2 hours. The reaction mixture was poured into a cooled 5% aqueous sodium chloride solution and extracted twice with ethyl acetate, and the extract solution was washed twice with a 5% aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent; ethyl acetate:n-hexane=5:95) to obtain 16.4 g of ethyl 4-(2-ethoxycarbonylphenyloxy)butyrate.

1. additionby adding dropwise
2. stirringThe reaction mixture was stirred at room temperature for 4.5 hours
3. waitat 65-70° C. for 2 hours
4. extractionextracted twice with ethyl acetate
5. washthe extract solution was washed twice with a 5% aqueous sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. customthe resulting residue was purified by a silica gel column chromatography (eluent; ethyl acetate:n-hexane=5:95)

ORD record

ord-877e9b09da9c48c7aa431588aa4bf424

Source dataset

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06369110B1