HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 22479176, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 22479124 | HCID 22479124 | — |
| Product | HCID 22479176 | HCID 22479176 | — |
Reaction Steps
A mixture of the compound from Example 139 (20 mg) and aqueous HBr (5 mL) was heated under reflux for 40 minutes. EtOAc was added and the organic layer was separated. The aqueous layer was extracted with EtOAC. The combined organic layers were dried over Na2SO4, filtered and evaporated. The residue was purified by preparative TLC (EtOAc). The obtained material was dissolved in MeOH (2 mL) and few drops of SOCl2 were added. The reaction mixture was heated under reflux for 1 hour. The residue was partitioned between EtOAc and water. The organic layer was dried over Na2SO4, filtered and concentrated. The product was purified via preparative TLC. MS m/z 449 (MH+). mp. 105.3° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06897225B1 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-497d8ca6faff49d7b2f95e53da832d53 |
| Source note | uspto-grants-2005_05 |