HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → 3-(4-Imidazol-1-ylmethylphenyl)-5-butyl-N-tert-butylthiophene-2-sulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-(4-Bromobenzyl)-1H-imidazole | HCID 2989557 | — |
| Reactant | 5-Butyl-2-(N-tert-butylaminosulfonyl)thiophene-3-boronic acid | HCID 11993911 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-(4-Imidazol-1-ylmethylphenyl)-5-butyl-N-tert-butylthiophene-2-sulfonamide | HCID 11994031 | — |
Reaction Steps
5-Butyl-2-(N-tert-butylaminosulfonyl)thiophene-3-boronic acid (300 mg, 1.27 mmol, see step (b) above), 1-(4-bromobenzyl)-1H-imidazole (606 mg, 1.90 mmol, see Example 1(d) above), toluene (15 mL), ethanol (4 mL), NaOH (1.0 M, 4.0 mL, 5.1 mmol) and Pd(PPh3)4 (43.9 mg, 0.038 mmol) were mixed under N2. The mixture was warmed to reflux for 2 hours, diluted with EtOAc (50 mL), washed with water and brine, and dried over MgSO4. The solvent was removed and the residue was separated by column chromatography using chloroform:methanol (20:1) as eluent. The product was not completely pure but was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652054B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-c5b77360ea354b6ab0a8adb32eb04ec3 |
| Source note | uspto-grants-2010_01 |