HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butanol → 1,4-Bis(4-bromophenyl)-1,4-butanedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | 4-Bromophenacyl bromide | HCID 7454 | — |
| Reactant | p-Bromoacetophenone | HCID 7466 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 1,4-Bis(4-bromophenyl)-1,4-butanedione | HCID 219217 | 39.1% |
Reaction Steps
To a solution of zinc(II) chloride (19.62 g, 144 mmol) in benzene (108 mL) were added diethylamine (11.16 mL, 108 mmol) and 2-methylpropan-2-ol (10.32 mL, 108 mmol) and the mixture was stirred at room temperature for 2 h. 2-bromo-1-(4-bromophenyl)ethanone (20.0 g, (72 mmol) and 1-(4-bromophenyl)ethanone (21.48 g, 108 mmol) were added in one portion, and the mixture was stirred overnight (18 h). Quenched with 5% H2SO4 (500 mL) and stirred vigorously to induce precipitation of the product, which was collected by vacuum filtration and washed with benzene, water, methanol, then dichloromethane, successively. The product was dried under vacuum to give the title compound as a white solid (11.15 g, 39.1% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691938B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-84be4a66095f43008dece16d3ab22995 |
| Source note | uspto-grants-2014_04 |