HCID 23434124, compound → HCID 23434089, compound

Temperature

0 °C

To a stirred solution of 3-(2,5-dichloro-3-thienyl)propanoic acid (0.225 g) in Et2O (5 mL) was added 1.05M MeLi in Et2O (2.0 mL) at 0° C. under nitrogen. After stirring at 0° C. for 30 minutes, the mixture was warmed to room temperature and stirred for 1 hour. The reaction was quenched by the addition of phosphate buffer solution (pH=7), and the resulting mixture was extracted with Et2O (30 mL). The organic layer was washed with water, brine, dried over MgSO4, and concentrated in vacuo. Chromatographic purification of the residue eluting with hexane-ethyl acetate (4:1) to give the title compound (0.173 g).

1. temperaturethe mixture was warmed to room temperature
2. stirringstirred for 1 hour
3. customThe reaction was quenched by the addition of phosphate buffer solution (pH=7)
4. extractionthe resulting mixture was extracted with Et2O (30 mL)
5. washThe organic layer was washed with water, brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customChromatographic purification of the residue
9. washeluting with hexane-ethyl acetate (4:1)

ORD record

ord-f1c1bac97fa340dca56f5dddf3c7e899

Source dataset

uspto-grants-2004_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06696470B2