Hydrochloric Acid → HCID 54457172, compound

To a stirred solution of trans-4-ethoxycarbonyl-2-methylthiomethyltetrahydrothiophene (compound No. 18-1, 307 mg) in methanol (10 ml), 1N sodium hydroxide solution (2.8 ml) was added under nitrogen atmosphere and the mixture was stirred for 1 hour at room temperature. The mixture was acidified with 1N hydrochloric acid and concentrated in vacuo. Saturated aqueous sodium chloride solution was added to the aqueous residue and extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo. The oily residue was purified by a silica gel column chromatography to give 260 mg (85%) of the titled compound (compound No. 19-1).

1. concentrationconcentrated in vacuo
2. additionSaturated aqueous sodium chloride solution was added to the aqueous residue
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with water and saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe oily residue was purified by a silica gel column chromatography

ORD record

ord-b89499f581eb4878907430b52090fecc

Source dataset

uspto-grants-1994_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05292767