HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 14953103, compound → HCID 14953107, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 14953103 | HCID 14953103 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrogen Bromide | HCID 260 | — |
| Product | HCID 14953107 | HCID 14953107 | 20.8% |
Reaction Steps
2 g of 4-[1-(4-methoxybenzyl)benzimidazol-2-yl]-3,3-dimethylbutanoic acid, prepared in Example 68, are dissolved in 40 ml of acetic acid and 40 ml of 48% hydrobromic acid. The mixture is refluxed for 3 hours and the solvents are evaporated off under vacuum. The residue is taken up with a 1 N solution of sodium hydroxide so as to adjust the pH to 9-10, and the resulting aqueous phase is washed with ether and then acidified with sulfur dioxide to pH 5.5. The crystals obtained are filtered off, washed with water and then with ether and then chromatographed on silica gel in a 9:1 chloroform/methanol eluent to give 0.4 g of 4-[1-(4-hydroxybenzyl)benzimidazol-2-yl]-3,3-dimethylbutanoic acid in the form of crystals melting at 215°-216° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05128359 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-6f6a6a5c793b4533b1d258a40d63985b |
| Source note | uspto-grants-1992_07 |