HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Bromobenzyl bromide → 3-[3-(2-Bromobenzyl)-3H-imidazol-4-yl]propionic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Bromobenzyl bromide | HCID 76965 | — |
| Reactant | Methyl 3-(1-Tritylimidazol-4-yl) Propionate | HCID 10475868 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-[3-(2-Bromobenzyl)-3H-imidazol-4-yl]propionic acid methyl ester | HCID 58827130 | — |
Reaction Steps
To a solution of 3-(1-trityl-1H-imidazol-4-yl)propanoic acid methyl ester (5.0 g, 12.6 mmol) in CH3CN (80 mL) is added a solution of 2-bromobenzylbromide (2.84 g, 11.4 mmol) in CH3CN (20 mL). The resulting clear solution is stirred at ambient temperature over the weekend. The mixture is concentrated and the remaining oil is taken up in 85 mL methanol and heated up at 70° C. for 2 h. Then the mixture is concentrated to give a yellow oil, which is taken up in EtOAc and washed with saturated aqueous NaHCO3 and brine, dried over anhydrous Na2SO4, and concentrated to yield a viscous oil. The crude reaction mixture is subjected to flash chromatography (silica gel) eluting with MeOH:CH2Cl2 to give the desired compound. MS (ESI) m/z 323 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835646B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-b41e2132a9a845cb9b032efa260435e5 |
| Source note | uspto-grants-2014_09 |