HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-Bromo-2-(methoxymethoxy)benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Bromophenol | HCID 7244 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Bromomethyl methyl ether | HCID 83093 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-Bromo-2-(methoxymethoxy)benzene | HCID 11310479 | 53.1% |
Reaction Steps
To a stirring suspension of sodium hydride (1.2 g, 52.1 mmol, 60% dispersion in mineral oil) in DMF (75 mL) at 0° C. was added 2-bromophenol (6.0 g, 34.7 mmol) dropwise. After stirring for 20 min, bromomethyl methyl ether (4.3 g, 34.7 mmol) was added. After stirring for 16 h at room temperature, the mixture was poured into water (250 mL) and extracted with hexane. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated. The residue was purified by column chromatography (silica gel, hexane) to yield the title compound as a colorless oil (4.0 g, 53%). 1HNMR (400 MHz, CDCl3) δ7.55 (d, 1H), 7.28 (t, 1H), 7.16 (d, 1H), 6.91 (t, 1H), 5.25 (s, 2H), 3.54 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331542B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-f6319eaf11314d858fc7d006bdb61eff |
| Source note | uspto-grants-2001_12 |