Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4'-Bromomethylbiphenyl-2-sulfonic acid dimethylaminomethylenamide | HCID 54161706 | — |
| Reactant | HCID 178441882 | HCID 178441882 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67561440 | HCID 67561440 | — |
Reaction Steps
5 g de 2-butyl 4-(methylthio) 1H-imidazole is dissolved in 120 cm3 of THF. Then 1.55 g of sodium hydride at 50% dispersion in oil is added slowly to the orange-coloured solution obtained. The temperature increases to 25° C. Agitation is carried out for 30 minutes at this temperature then 14 g of 4'-bromomethyl N-[(dimethylamino) methylene](1,1'-biphenyl) 2-sulphonamide is introduced. Agitation is carried out at ambient temperature until evolution ends, i.e. for approximately 3 hours, followed by taking up in water, extracting with ethyl acetate, separating by chromatography on silica eluting with ethyl acetate then impasting in iso ether, filtering and drying. In this way 9.35 g of expected product (colourless crystals) is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05807878 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-6b7de749a960459891e492e87a192d55 |
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| Source note | uspto-grants-1998_09 |
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