HuagongsheHuagongshe Chemistry Print Report · For research reference only
Catechol → 2,2-Dimethyl-1,3-benzodioxole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Catechol | HCID 289 | — |
| Reactant | 2,2-Dimethoxypropane | HCID 6495 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2,2-Dimethyl-1,3-benzodioxole | HCID 285869 | 18.9% |
Reaction Steps
A mixture of catechol (10 g, 91 mmol), 2,2-Dimethoxypropane (8.6 g, 82.6 mmol) and p-TsOH (33 mg, 0.17 mmol) in toluene (100 ml) was stirred at reflux for 6 h. After reaction, the mixture was cooled to room temperature and NaHCO3 was added to neutralize the mixture. The solvent was removed and the residue was purified by distillation under reduced pressure at 36° C. to obtain 2,2-dimethylbenzo[d][1,3]dioxole (2.34 g, 17%) as a yellow oil. 1H NMR (CDCl3-d6) δ 1.69 (s, 6H), 6.78 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040556B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-161986bb6e864884bb43625a9a06bb2a |
| Source note | uspto-grants-2015_05 |