HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178524215, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86657758 | HCID 86657758 | — |
| Solvent | Hydrogen Bromide | HCID 260 | — |
| Product | HCID 178524215 | HCID 178524215 | — |
Reaction Steps
A solution of 11a (240 mg, 0.527 mmol) in hydrobromic acid (5.00 mL of a 33 wt. % acetic acid solution) was heated to 60° C. in a sealed tube. After 20 h, the reaction mixture was cooled to rt and was added to said. aq. NaHCO3. The resulting mixture was extracted with EtOAc, and combined organics were concentrated in vacuo to give a crude residue that was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (CH3CN/H2O as eluent, 0.05% TFA as modifier), followed by lyophilization of the purified fractions to afford the title compound 11b. m/z (ES) 428 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367679B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-761424738be449b58716bffff20c202c |
| Source note | uspto-grants-2013_02 |