HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dibromoethane → HCID 11637164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dibromoethane | HCID 7839 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 2,3-dihydroxy-4-methoxybenzoate | HCID 11694090 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11637164 | HCID 11637164 | 81.3% |
Reaction Steps
A mixture of methyl 2,3-dihydroxy-4-methoxybenzoate (0.176 mol), 1,2-dibromo-ethane (0.282 mol), K2CO3 (0.444 mol) and CuO (1.4 g) in DMF (1000 ml) was stirred for 6 hours, cooled, filtered and the filtrate was evaporated. Water (300 ml) was added. The mixture was extracted twice with DCM (300 ml). The organic layer was separated, washed with a saturated NaHCO3 solution, dried, filtered and the solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 32.1 g of methyl 2,3-dihydro-8-methoxy-1,4-benzodioxin-5-carboxylate (intermediate 1, mp. 84° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07635706B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-3dec537237794b5d927b08d75911c7ef |
| Source note | uspto-grants-2009_12 |