Hydrochloric Acid → HCID 68285893, Verbindung

Temperatur

75 °C

Ethyl 5-(4-chlorophenyl)-4-methyl-3-(3-methyl-4-sulfamoylphenyl)thiophene-2-carboxylate (41c, 0.6 g, 1.33 mmol) was suspended in ethanol (20 ml) and a solution of sodiumhydroxide (0.1 g, 2.66 mmol) in water (2 ml] was added to it at 25° C. The reaction mixture was then heated at 75° C. under stirring for 2 hours. The progress of the reaction was monitored by TLC. The reaction mixture was concentrated under reduced pressure. The residue so obtained was then diluted with water (5 ml) and the mixture was cooled using ice bath. To the cooled mixture was added 10% aqueous HCl to bring the pH of the mixture between about 5 and 6. The mixture was then extracted with ethyl acetate (2×35 ml). The combined organic layer was then dried over anhydrous Na2SO4. The solvent was evaporated from the dried organic layer under reduced pressure to obtain the title compound (0.53 g, 94%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customThe residue so obtained
3. temperaturethe mixture was cooled
4. extractionThe mixture was then extracted with ethyl acetate (2×35 ml)
5. dry with materialThe combined organic layer was then dried over anhydrous Na2SO4
6. customThe solvent was evaporated from the dried organic layer under reduced pressure

ORD-Eintrag

ord-acfb0b6444bc4c30b5ccb29cc7e537e6

Quelldatensatz

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09393247B2