Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 18920656 | HCID 18920656 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 18920664 | HCID 18920664 | 69.1% |
Reaction Steps
A mixture of 1,2-di(p-bromophenyl)-hydroxyethane (7.2 g, 0.02 mol), acetic anhydride (20 mL, 0.2 mol), pyridine (20 mL) was stirred at 60° C. for 30 min. The solution was then allowed to stand at room temperature for 2 days. The mixture was poured into ice water (250 g) and extracted with methylene chloride (150 mL). The organic phase was extracted with 5% aqueous sodium carbonate (100 mL×2), 5% aqueous hydrochloric acid (100 mL×2), water (100 mL×2), dried over sodium sulfate and concentrated to give an oil (5.5 g) which solidified upon standing. This was purified by passing through a short alumina column followed by recrystallization from hexanes to give the above white solid product (4.2 g): mp: 61-64° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05753757 |
|---|
| Source dataset | uspto-grants-1998_05 |
|---|
| ORD ID | ord-a9fc0a8c112f4970a28aa3e8f47e11c4 |
|---|
| Source note | uspto-grants-1998_05 |
|---|