Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-Chloroethyl Cyclohexyl Carbonate | HCID 11229529 | — |
| Edukt | HCID 66758670 | HCID 66758670 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 66757832 | HCID 66757832 | 116,7% |
Reaktionsschritte
To a solution of product of example 118 (1.1 g) in dimethylformamide (15 ml) were added sodium iodide (0.17 g), potassium carbonate (0.38 g) and cyclohexyl 1-chloroethyl carbonate (J. Antibiotics, 1987, 40, 81.) (0.57 g) at room temperature. The mixture was stirred at 70° C. for 1 hour. Water and ethyl acetate were added to the reaction mixture, the organic layer was separated and washed with saturated aqueous sodium chloride, and dried with magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate:methanol=100:3). The obtained oil was dissolved with ethyl acetate, and 4 N hydrochloric acid ethyl acetate solution (0.8 ml) was added. The precipitation was filtered to give the titled compound (0.96 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08653096B2 |
|---|
| Quelldatensatz | uspto-grants-2014_02 |
|---|
| ORD ID | ord-2299faa76a544790bfbdd76da71e923f |
|---|
| Quellennotiz | uspto-grants-2014_02 |
|---|