HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → 1-(Bromomethyl)-2,5-dimethoxy-3,4,6-trimethylbenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | (2,5-Dimethoxy-3,4,6-trimethylphenyl)methanol | HCID 13389492 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(Bromomethyl)-2,5-dimethoxy-3,4,6-trimethylbenzene | HCID 14277760 | 119.9% |
Reaction Steps
A solution of 16.5 g (78.5 mmol) of 2,5-dimethoxy-3,4,6-trimethylbenzylalcohol in 90 ml of tetrahydrofuran was cooled to 0° C., to which 14.2 g (52.5 mmol) of phosphorus tribromide was added with stirring. After stirring at the same temperature for 30 minutes, the reaction mixture was diluted with water and extracted with isopropyl ether. The extract was washed with a saturated aqueous solution of sodium hydrogen carbonate and dried, from which the solvent was evaporated off. The residue was crystallized from methanol, to give 17.2 g (80.0%) of 2,5-dimethoxy-3,4,6-trimethylbenzyl bromide. m.p. 71°-72° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04985447 |
| Source dataset | uspto-grants-1991_01 |
| ORD ID | ord-db2092a3413d4ba3a8ec55ba72e0ab1c |
| Source note | uspto-grants-1991_01 |