HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 20189570, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Chlorodifluoromethane | HCID 6372 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 2,3-Dimethoxyphenol | HCID 78828 | — |
| Catalyst | HCID 131715232 | HCID 131715232 | — |
| Solvent | Cyclohexane ethylacetate | HCID 21867204 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 20189570 | HCID 20189570 | 48% |
Reaction Steps
50 g of 2,3-dimethoxyphenol are reacted analogously to Example B12a with 80 g of potassium hydroxide and chlorodifluoromethane in dioxane/water. The mixture is extracted with diisopropyl ether by shaking, the extract is washed with sodium hydroxide solution and 35 g of a product (b.p. 70°-74° C./0.3 mbar) are obtained which is reacted with 100% nitric acid analogously to Example B7b. The reaction product is subjected to chromatography on a silica gel column with cyclohexane/ethyl acetate (3:2), after which 1-difluoromethoxy-2,3-dimethoxy-5-nitrobenzene (m.p. 72°-73° C.) is isolated in 48% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04686230 |
| Source dataset | uspto-grants-1987_08 |
| ORD ID | ord-0b49246c61754d2eb5f40629087f96d0 |
| Source note | uspto-grants-1987_08 |