Acetic Acid → HCID 59303954, compound

3-Butoxymethylthiophene (6.17 grams, 36.24 mmol) was dissolved in 100 milliliters of CH2Cl2, and then 100 milliliters of acetic acid (AcOH) were added. N-Bromosuccinimide (NBS) (6.45 grams, 36.24 mmol) was then added in portions to the resulting mixture under stirring. The mixture resulting was then stirred at room temperature, about 23° C. to about 27° C., for 24 hours. Reaction completion was determined by 1H NMR. The solvents were then removed by evacuation. The residue remaining was dissolved in hexane, and the soluble part was passed through a short silica gel column (10 centimeters×3 centimeters). After removing the solvent, the resulting colorless liquid was purified by column chromatography using hexane/CH2CI2 (3/2, v/v) then by distillation under reduced pressure.

1. customThe mixture resulting
2. stirringwas then stirred at room temperature, about 23° C. to about 27° C., for 24 hours
3. customReaction completion
4. customThe solvents were then removed by evacuation
5. dissolutionThe residue remaining was dissolved in hexane
6. customAfter removing the solvent
7. customthe resulting colorless liquid was purified by column chromatography
8. distillationv/v) then by distillation under reduced pressure

ORD record

ord-aabdb25faee34766b22ffc1dda43a448

Source dataset

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07718999B2