HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → 6-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 5-Bromo-2-hydroxybenzyl alcohol | HCID 75342 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | 2,2-Dimethoxypropane | HCID 6495 | — |
| Product | 6-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine | HCID 14520338 | — |
Reaction Steps
To 5-bromo-2-hydroxybenzyl alcohol (93 g, 0.46 mol, available from Sigma-Aldrich) in 2.0 L of 2,2-dimethoxypropane was added 700 mL of acetone, followed by zinc chloride (170 g). After stirring for 18 hours, 1.0 M aqueous sodium hydroxide was added until the aqueous phase was basic. Diethyl ether (1.5 L) was added to the slurry and the organic phase was decanted into a separatory funnel. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07732441B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-20446c10caf4475b83f552e064cafc91 |
| Source note | uspto-grants-2010_06 |