HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 6-Bromo-3,4-dimethoxybenzaldehyde | HCID 79351 | — |
| Reactant | Methylorthoformate | HCID 53629101 | — |
| Product | 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene | HCID 11077146 | 93.9% |
Reaction Steps
6-Bromo-3,4-dimethoxybenzaldehyde (470 g) is suspended in methanol (600 ml), and thereto are added methyl ortho-formate (1025 ml) and IRA-120 (H+-type) (10 g), and the mixture is refluxed for one hour. The mixture is cooled to room temperature, and the insoluble materials are removed by filtration. The filtrate is concentrated under reduced pressure, and the resulting residue is dissolved in diethyl ether. The mixture is washed, dried, and evaporated to remove the diethyl ether. The resulting residue is distilled under reduced pressure to give 6-bromo-3,4-dimethoxybenzaldehyde dimethylacetal (522 g) as main distillate (133°-138° C./1Torr).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05342941 |
| Source dataset | uspto-grants-1994_08 |
| ORD ID | ord-ffc0aa98115c465a825610873af9afdf |
| Source note | uspto-grants-1994_08 |