HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Aminosalicylic acid → HCID 66799978, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Aminosalicylic acid | HCID 68443 | — |
| Reactant | 5-Chloro-3-methylbenzo(b)thiophene-2-sulfonyl chloride | HCID 2735756 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 66799978 | HCID 66799978 | 72% |
Reaction Steps
A solution of 5-chloro-3-methyl-benzothiophene-2-sulfonyl chloride (17 mg, 0.060 mmol) and 3-aminosalicylic acid (14 mg, 0.090 mmol) in 1200 μL of water/dioxane (1:6) was shaken at 35° C. for 5 days. The product was purified by reversed phase chromatography (ACE C8, 4 μm, 21×50 mm, flow 25 ml/min, gradient: 0.1% TFA in water/MeCN over 6 minutes). The title compound was obtained in 72% yield (17.2 mg). 1H NMR (500 MHz, DMSO-d6) δ ppm 2.48 (s, 3 H) 6.85 (t, J=7.92 Hz, 1 H) 7.46 (dd, J=7.69, 1.64 Hz, 1 H) 7.55 (dd, J=8.66, 2.05 Hz, 1 H) 7.63 (dd, J=7.92, 1.64 Hz, 1 H) 8.00 (dd, J=2.05, 0.47 Hz, 1 H) 8.04 (dd, J=8.66, 0.47 Hz, 1 H) 10.17 (br. s., 1 H). MS (ESI+) m/z 398 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09233946B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-a989e8caea2847b395e4000d2baf39c3 |
| Source note | uspto-grants-2016_01 |