HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → 6-(4-Bromo-phenylamino)-7-chloro-3H-benzoimidazole-5-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 7-Chloro-6-phenylamino-3H-benzoimidazole-5-carboxylic acid methyl ester | HCID 86599017 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-(4-Bromo-phenylamino)-7-chloro-3H-benzoimidazole-5-carboxylic acid methyl ester | HCID 66898342 | 54.7% |
Reaction Steps
7-Chloro-6-phenylamino-3H-benzoimidazole-5-carboxylic acid methyl ester 7c (0.327 g, 1.08 mmol) is dissolved into DMF (16 mL) and NBS (0.193 g, 1.08 mmol) is added. After one hour, the reaction mixture is quenched by the addition of saturated aqueous NaHSO3. The reaction mixture is then partitioned between EtOAc/THF and water. The organic layer is washed with water and brine. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure. The recovered solid is triturated with ether to give 0.225 g (54%) pure desired product. MS ESI (+) m/z 382, 384 (M+, Br pattern) detected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07425637B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-d815b576b31b461cbf515169d6b039d5 |
| Source note | uspto-grants-2008_09 |