HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Iodide → HCID 18982209, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,4-Benzodioxin, 5-(2-chloroethoxy)-2,3-dihydro- | HCID 11469956 | — |
| Reactant | HCID 18982196 | HCID 18982196 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl ketone | HCID 7288 | — |
| Solvent | Acetone diethylether | HCID 21584533 | — |
| Product | HCID 18982209 | HCID 18982209 | — |
Reaction Steps
A mixture of 5 g of 5-(2-chloroethoxy)-1,4-benzodioxane, 7.8 g of 4-(4-fluorobenzoyl)perhydroazepine hydrobromide (described in Patent EP 389,352), 1 g of potassium iodide and 6.5 g of potassium carbonate in 100 ml of diethyl ketone is maintained at 100 C. for 24 hours. The inorganic salts are then filtered off and the filtrate is concentrated under vacuum. The residue is purified by chromatography on a column of silica, with a dichloromethane/methanol/aqueous ammonia (97/3/0.3) eluent mixture. The base obtained is salified with hydrochloric methanol in an acetone/ether mixture. Melting point: 106°-107° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05500443 |
| Source dataset | uspto-grants-1996_03 |
| ORD ID | ord-0d2c21b63c4a43dab9d4913c9d180fc0 |
| Source note | uspto-grants-1996_03 |