HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → (1-Hydroxy-cyclohexyl)-acetic acid ethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Ethyl bromoacetate | HCID 7748 | — |
| Edukt | Cyclohexanone | HCID 7967 | — |
| Katalysator | Zinc | HCID 23994 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (1-Hydroxy-cyclohexyl)-acetic acid ethyl ester | HCID 219250 | 95,2% |
Reaktionsschritte
To a solution of cyclohexanone (9.52 g, 97.0 mmol), a zinc powder (7.6 g, 116.4 mmol) and a small amount of iodine in THF (100 ml) was added dropwise ethyl bromoacetate (11.8 ml, 106.7 mmol) under a nitrogen atmosphere, and the mixture was heated under reflux for 5 hrs. 10% Sulfuric acid (100 ml) was carefully added under ice-cooling, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4, and concentrated under reduced pressure to give the title compound (17.2 g, 94%) as a colorless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07943770B2 |
| Quelldatensatz | uspto-grants-2011_05 |
| ORD ID | ord-d2e026c0189145f6877d14a4e2913dec |
| Quellennotiz | uspto-grants-2011_05 |