Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 71203615 | HCID 71203615 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 71203616 | HCID 71203616 | 90.5% |
Reaction Steps
Methyl 5-(6-methoxy-4′-sulfamoyl-[1,1′-biphenyl]-3-yl)-3,4-dimethylthiophene-2-carboxylate (step-5, 0.2 g, 0.45 mmol) was suspended in ethanol (10 ml). Aqueous solution of NaOH (0.09 g. 2.24 mmol in water 2 ml) was added to the reaction mixture at 0° C. The reaction mixture was heated at 80° C. under stirring for 1.5 hour. The progress of the reaction was monitored by TLC. The reaction mixture was then concentrated under reduced pressure. Dilute hydrochloric acid was added to the separated aqueous layer to bring the pH of the solution to between 6 and 7. The resulting mixture was extracted with ethyl acetate (2×25 ml). The combined organic layer was dried over anhydrous Na2SO4. The solvent was evaporated from the dried organic layer under reduced pressure to obtain the title compound 9f (0.17 g, 86.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08946432B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-4e075b51bce34a92836d0224ea3c668e |
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| Source note | uspto-grants-2015_02 |
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