HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-(Bromomethyl)-1,2,3-trimethoxybenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | 3,4,5-Trimethoxybenzyl alcohol | HCID 77449 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-(Bromomethyl)-1,2,3-trimethoxybenzene | HCID 10355271 | 86.7% |
Reaction Steps
Dissolving 3,4,5-trimethoxyl benzyl alcohol (14.05 g, 70.89 mmol) in dichlormethane (100 ml) in a three-necked bottle (250 ml); dissolving phosphorus tribromide (6.73 ml, 70.89 mmol) in dichlormethane (25 ml) for it to react at room temperature for 50 minutes, cooling in refrigeratory, slowly adding deionized water (18 ml, 1.0 mol) dropwise to quench, washing with deionized water (100 ml) twice, drying with anhydrous magnesium sulfate, filtering, washing the filter residue with dichlormethane (20 ml), conflating the filtrate, concentrating in rotarory evaporater, and vacuum drying to get 3,4,5-trimethoxyl benzyl bromine (16.05 g of faint yellow solid), yield: 84.44%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897820B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-4f37dd3764f74a11a1f60302287f661d |
| Source note | uspto-grants-2011_03 |