HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → N-(1,1-Dimethylethyl)-4-[5-(3-fluoro-4-methoxyphenyl)-1H-imidazol-1-yl]benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Tosylmethyl isocyanide | HCID 161915 | — |
| Reactant | N-tert-Butyl-4-((3-fluoro-4-methoxybenzylidene)amino)benzenesulfonamide | HCID 11132250 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | N-(1,1-Dimethylethyl)-4-[5-(3-fluoro-4-methoxyphenyl)-1H-imidazol-1-yl]benzenesulfonamide | HCID 11784436 | 90% |
Reaction Steps
A mixture of N-tert-butyl-4-[(3-fluoro-4-methoxybenzylidene)amino]benzenesulfonamide (41.5 g, 114 mmol, obtained in example 2), tosylmethylisocyanide (33.22 g, 171 mmol), K2CO3 (31.1 g, 228 mmol), DME (340 mL) and MeOH (778 mL) is heated at reflux for 3 h. The solvent is removed and the residue is taken up in a CHCl3/H2O mixture and the layers are separated. The aqueous phase is extracted with CHCl3 and the combined organic extracts are dried over MgSO4 and concentrated. A crude product is obtained, which is washed with Et2O several times to give 41.40 g of a creamy solid that is directly used in the next reaction (yield: 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476456B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-c567a15dfeef4be1b26c2c5d4ade956e |
| Source note | uspto-grants-2013_07 |