HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Bromo-2-methyl-1H-benzo[d]imidazole → HCID 58107460, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Bromo-2-methyl-1H-benzo[d]imidazole | HCID 610979 | — |
| Reactant | 4-chloro-N-methoxy-N-methyl-3-sulfamoyl-benzamide | HCID 58107399 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58107460 | HCID 58107460 | — |
Reaction Steps
A solution of 0.303 g of 6-bromo-2-methyl-1H-benzoimidazole in tetrahydrofuran (20 mL) is cooled to −50° C. and treated with 2.7 mL of tert-butyllithium (1.5 M in pentane). After 2 h at −50° C. the reaction mixture is treated with 0.12 g of 4-chloro-N-methoxy-N-methyl-3-sulfamoyl-benzamide in tetrahydrofuran (10 mL). After 3 h the mixture is quenched with saturated aqueous ammonium chloride, taken up in ethyl acetate, and washed with saturated aqueous sodium chloride. The organics are dried (magnesium sulfate), concentrated and purified by silica gel chromatography (98:2 methylene chloride/methanol) to give 2-chloro-5-(2-methyl-3H-benzoimidazole-5-carbonyl)-benzenesulfonamide. MS (m/z): 348 (M−1); Rf 0.30 (9:1 methylene chloride/methanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975439B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-8341fc17a26b4d9ca2143b996f11b4ea |
| Source note | uspto-grants-2015_03 |