Potassium Carbonate → HCID 67959076, compound

Temperature

85 °C

A solution of methyl 4-bromo-3-hydroxythiophene-2-carboxylate (53.0 g), potassium carbonate (46.2 g), 2-bromoacetamide (37.0 g) and DMF (500 ml) was stirred at 60° C. for 2 hr, and the solvent was evaporated under reduced pressure. Water (300 ml) was added to the residue, and the solid was collected by filtration. To the obtained solid were added potassium carbonate (61.6 g), water (20 ml) and MeOH (500 ml, and the mixture was stirred at 85° C. for 1 hr. After cooling to room temperature, the solid were collected by filtration. The obtained solid was dissolved in water (300 mL), and the mixture was adjusted with 6 N hydrochloric acid to pH 3. The obtained solid was collected by filtration, and washed with water to give the title compound (50.5 g, 80.8%) as a solid.

1. customthe solvent was evaporated under reduced pressure
2. additionWater (300 ml) was added to the residue
3. filtrationthe solid was collected by filtration
4. additionTo the obtained solid were added potassium carbonate (61.6 g), water (20 ml) and MeOH (500 ml
5. temperatureAfter cooling to room temperature
6. filtrationthe solid were collected by filtration
7. dissolutionThe obtained solid was dissolved in water (300 mL)
8. filtrationThe obtained solid was collected by filtration
9. washwashed with water

ORD record

ord-cffbdc54f21d44c79ddaf8eb8cc1c2d0

Source dataset

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08916549B2