HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-2-methylpropane → 7-iodo-3-isobutyl-3H-benzoimidazole-5-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-2-methylpropane | HCID 6555 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1H-Benzimidazole-5-carboxylic acid, 7-iodo-, methyl ester | HCID 59627771 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 7-iodo-3-isobutyl-3H-benzoimidazole-5-carboxylic acid methyl ester | HCID 59627773 | 87% |
| Product | 7-iodo-1-isobutyl-1H-benzoimidazole-5-carboxylic acid methyl ester | HCID 67516669 | 11% |
Reaction Steps
To a solution of 7-iodo-3H-benzoimidazole-5-carboxylic acid methyl ester (783 mg, 2.59 mmol) in DMF (50 mL) was added Cs2CO3 (1.69 g, 5.18 mmol), followed by isobutyl bromide ((0.338 mL, 3.11 mmol). The reaction mixture was stirred room temperature overnight, then partitioned between water and ethyl acetate. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure. Purification of the residue by column chromatography gave 805 mg (87%) of 7-iodo-3-isobutyl-3H-benzoimidazole-5-carboxylic acid methyl ester (the regioisomer 7-iodo-1-isobutyl-1H-benzoimidazole-5-carboxylic acid methyl ester (100 mg, 11%) was recovered as separate fraction).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476457B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-8f462924085c4597a826d64dbb56b9ee |
| Source note | uspto-grants-2013_07 |