HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 1-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethoxy)-naphthalene-2-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-Naphthalenecarboxylic acid, 1-hydroxy-, methyl ester | HCID 70358 | — |
| Reactant | 2-Bromomethyl-1,4-benzodioxane | HCID 98333 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethoxy)-naphthalene-2-carboxylic acid methyl ester | HCID 66701207 | 55.2% |
Reaction Steps
To 4.19 g cesium carbonate and 1.37 g methyl 1-hydroxy-2-naphthoate in 25 ml abs. DMF was added 1.62 g 2-bromomethyl-2,3-dihydro-benzo[1,4]dioxine and the mixture was reacted for 16 h at 50° C. The reaction was poured unto ice, the resulting precipitate was isolated by filtration, dissolved in ethyl acetate and washed with brine. The organic phase was dried over magnesium sulphate and concentrated in vacuo. The resulting residue was purified by flash chromatography (silica, heptane/ethyl acetate) to yield 1.31 g of 1-(2,3-dihydro-benzo[1,4]dioxin-2-ylmethoxy)-naphthalene-2-carboxylic acid methyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919628B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-a66146e51e9440f49a657fc8c977e4ac |
| Source note | uspto-grants-2011_04 |